WO2022232905A1 - Industrial hashish and method for producing same at an industrial scale - Google Patents

Industrial hashish and method for producing same at an industrial scale Download PDF

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Publication number
WO2022232905A1
WO2022232905A1 PCT/CA2022/050624 CA2022050624W WO2022232905A1 WO 2022232905 A1 WO2022232905 A1 WO 2022232905A1 CA 2022050624 W CA2022050624 W CA 2022050624W WO 2022232905 A1 WO2022232905 A1 WO 2022232905A1
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WIPO (PCT)
Prior art keywords
hashish
product
cannabis
trichomes
isolated
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PCT/CA2022/050624
Other languages
French (fr)
Inventor
Francois Chouinard
Jamie SAVARD
Renato Devien DURBANO
Original Assignee
Hexo Operations Inc.
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Publication date
Application filed by Hexo Operations Inc. filed Critical Hexo Operations Inc.
Priority to CA3217597A priority Critical patent/CA3217597A1/en
Publication of WO2022232905A1 publication Critical patent/WO2022232905A1/en

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Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • A24B15/16Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)

Definitions

  • This application generally relates to the field of industrial hashish products and methods of manufacturing hashish products at an industrial scale.
  • Hashish is a concentrated derivative of cannabis plants, the dried resin glands of the flowering tops of mature and unpollinated female cannabis plants.
  • the resin glands are known as trichomes. It contains the same active ingredients as the cannabis plants - including cannabinoids - yet at higher concentration levels than the un-sifted buds or leaves from which dried marijuana is made, which is tantamount to higher potency.
  • the cannabis trichomes are substantially isolated from cannabis plant matter.
  • the isolated cannabis trichomes are usually collected by hand, by mechanical beating of the cannabis plants or by submersing the cannabis plants in icy water and then using small sieves to isolate the cannabis trichomes.
  • mechanical isolation may be used to isolate cannabis trichomes from cannabis plant matter, such as sieving through a screen by hand (i.e. , dry sift) or in motorized tumblers, as described for example in WO 2019/161509.
  • Isolated cannabis trichomes have a powder appearance (typically referred to as “kief”) and are pressed to obtain blocks of hashish.
  • hashish is very labor intensive, and it is practically an art, where the skills of the individual play a key role in defining the quality and/or physical characteristics of the finished hashish product.
  • the consistency and appearance of hashish vary depending on the manufacturing process and amount of leftover plant material (e.g., chlorophyll). Consumers often associate the hash color or smell to quality and/or origin.
  • Good-quality pressed dry-sift hashish ranges in appearance from light blondish-brown, to greenish or dark-brown. Examples thereof include “Lebanese” hashish, which is from yellow to reddish, and “Moroccan” hashish which is from greenish to darker brown.
  • Hand-rubbed pressed hashish is most commonly referred to as being “Afghani” (from Afghanistan) or “Charas” (from India and Pakistan). This form of hashish is produced by rubbing the living plants to remove the sticky resin, which is then rolled into balls or eggs and left to cure before being consumed or sold. Hand-rubbed types of hash should be smooth, black or brownish- black, and often sticky to the touch. When opened, consumers expect the interior to be a delicate brown, perhaps with a slight green tinge (a very green interior indicates excessive residual plant material).
  • the present inventors have developed a hashish that matches the consumer appealing hand-made products where the manufacturing method can be at least partially automated and which does not require use of coloring agents or post-processing steps to artificially impart desired visual characteristics that are typically associated with good quality hashish.
  • the present disclosure relates to a process of making a hashish product, comprising providing isolated cannabis trichomes; mixing the isolated cannabis trichomes while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture; and retrieving at least a portion of the resinous mixture through an extrusion die to obtain the hashish product, wherein the hashish product is a substantially homogeneous cohesive mass of the isolated trichomes having a % reflectance of at least 4%85.
  • the process may include one or more of the following features:
  • the hashish product has a lightness value L* £ 50 on CIELAB scale, preferably from 0 to about 40, or of from about 10 to about 30, or of from about 15 to about 25.
  • the hashish product has a % reflectance of at least 4.5%85, at least 5%85, or at least 5.5%85.
  • the mixing includes applying compression and shear forces to the isolated trichomes via a plurality of interpenetrate helicoidal surfaces within an elongated enclosure.
  • the interpenetrate helicoidal surfaces are on at least two screws extending along at least a portion of a longitudinal axis of the elongated enclosure.
  • the rotational speed of the at least two screws is between about 10 rpm and about 1000 rpm, preferably between 100 rpm and 200 rpm.
  • said elongated enclosure comprises a plurality of sections corresponding to longitudinal segments of the at least two screws.
  • the temperature in each section of the plurality of sections is independently selected in the range of from about 20°C to about 170°C.
  • the plurality of sections includes at least one mixing section and at least one conveying section. • the at least one mixing section is maintained at a first temperature and the least one conveying section is maintained at a second temperature, the first and second temperatures being different.
  • the plurality of sections includes at least one reverse flow section.
  • At least a first section of the plurality of sections comprises a first inlet for providing the isolated trichomes.
  • At least a second section of the plurality of sections comprises a second inlet for providing one or more additional component(s).
  • the one or more additional component(s) include one or more cannabinoid, one or more terpene, one or more flavonoid, one or more flavoring agent, water, one or more non-toxic coloring agent, or a mixture thereof.
  • the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
  • the one or more cannabinoid(s) includes a plurality of cannabinoids.
  • the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
  • the cutting pattern includes cutting the hashish product along a transverse axis to obtain pieces thereof of identical length and/or weight.
  • the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%.
  • the isolated cannabis trichomes are from a single cannabis strain.
  • the isolated cannabis trichomes are from a plurality of cannabis strains.
  • the hashish product comprises a moisture content of from about 2 wt.% to about 8 wt.%, or of from about 2 wt.% to about 5 wt.%.
  • the present disclosure relates to a hashish product comprising a substantially homogeneous cohesive mass of isolated cannabis trichomes made by the process described above.
  • the present disclosure relates to a hashish product comprising a substantially homogeneous cohesive mass of isolated cannabis trichomes having a % reflectance of at least 4%85.
  • the hashish product may include one or more of the following features:
  • the hashish product has a lightness value L* £ 50 on CIELAB scale, or a lightness value L* from 0 to about 40, of from about 10 to about 30, of from about 15 to about 25.
  • the hashish product has a % reflectance of at least 4.5%85, at least 5%85, or at least 5.5%85.
  • the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
  • the one or more cannabinoid(s) includes a plurality of cannabinoids.
  • the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
  • the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%.
  • the isolated cannabis trichomes are from a single cannabis strain.
  • the isolated cannabis trichomes are from a plurality of cannabis strains.
  • the hashish product comprises a moisture content of from about 2 wt.% to about 8 wt.%, or of from about 2 wt.% to about 5 wt.%.
  • the present disclosure relates to process of making a hashish product, comprising providing isolated cannabis trichomes; mixing the isolated cannabis trichomes while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture; and retrieving at least a portion of the resinous mixture through an extrusion die to obtain the hashish product, wherein the hashish product has a moisture content of no more than about 8 wt.%.
  • the present disclosure relates to a process of making a hashish product, comprising providing isolated cannabis trichomes; mixing the isolated cannabis trichomes while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture; and retrieving at least a portion of the resinous mixture through an extrusion die to obtain the hashish product, wherein the hashish product is free of exogenous water.
  • the moisture content of the hashish product is at least 2 wt.%.
  • the hashish product has a lightness value L* £ 50 on CIELAB scale, preferably from 0 to about 40, or of from about 10 to about 30, or of from about 15 to about 25.
  • the hashish product has a % reflectance of at least 4%85.
  • the % reflectance of the hashish product is at least 4.5%85, at least 5%85, or at least
  • the mixing includes applying compression and shear forces to the isolated trichomes via a plurality of interpenetrate helicoidal surfaces within an elongated enclosure.
  • the interpenetrate helicoidal surfaces are on at least two screws extending along at least a portion of a longitudinal axis of the elongated enclosure.
  • the process further comprises adjusting a rotational speed of the at least two screws to obtain the resinous mixture.
  • the rotational speed of the at least two screws is between about 10 rpm and about 1000 rpm, preferably between 100 rpm and 200 rpm.
  • the elongated enclosure comprises a plurality of sections corresponding to longitudinal segments of the at least two screws.
  • the process further comprises controlling a temperature in at least one section of the plurality of sections.
  • the temperature in each section of the plurality of sections is independently selected in the range of from about 20°C to about 170°C.
  • the plurality of sections includes at least one mixing section and at least one conveying section.
  • the at least one mixing section is maintained at a first temperature and the least one conveying section is maintained at a second temperature, the first and second temperatures being different.
  • the plurality of sections includes at least one reverse flow section.
  • At least a first section of the plurality of sections comprises a first inlet for providing the isolated trichomes.
  • the one or more additional component(s) include one or more cannabinoid, one or more terpene, one or more flavonoid, one or more flavoring agent, one or more non-toxic coloring agent, or a mixture thereof.
  • the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
  • the one or more cannabinoid(s) includes a plurality of cannabinoids.
  • the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
  • the process further comprises cutting the hashish product according to a pre-established cutting operational parameter.
  • the cutting pattern includes cutting the hashish product along a transverse axis to obtain pieces thereof of identical length and/or weight.
  • the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%.
  • the isolated cannabis trichomes are from a plurality of cannabis strains.
  • the present disclosure relates to a hashish product comprising a substantially homogeneous cohesive mass of isolated cannabis trichomes made by one of the processes described above.
  • the present disclosure relates to a hashish product comprising an extruded, substantially homogeneous cohesive mass of isolated cannabis trichomes having a moisture content of no more than about 8 wt.%.
  • the present disclosure relates to a hashish product comprising an extruded, substantially homogeneous cohesive mass of isolated cannabis trichomes that is free of exogenous water during extrusion.
  • the hashish products may include one or more of the following features:
  • the moisture content of the hashish product is at least 2 wt.%.
  • the hashish product has a lightness value L* £ 50 on CIELAB scale, preferably from 0 to about 40, or of from about 10 to about 30, or of from about 15 to about 25.
  • the hashish product has a % reflectance of at least 4%85.
  • the % reflectance of the hashish product is at least 4.5%85, at least 5%85, or at least 5.5%85.
  • the hashish product comprises one or more additional component(s) selected from one or more cannabinoid, one or more terpene, one or more flavonoid, one or more flavoring agent, one or more non-toxic coloring agent, and any mixtures thereof.
  • the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
  • the one or more cannabinoid(s) includes a plurality of cannabinoids.
  • the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
  • the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%.
  • the isolated cannabis trichomes are from a single cannabis strain.
  • the isolated cannabis trichomes are from a plurality of cannabis strains.
  • FIG. 1 illustrates a non-limiting flowchart example of a process for making a hashish product in accordance with an embodiment of the present disclosure
  • FIG. 2 illustrates a non-limiting flowchart example of steps for obtaining isolated cannabis trichomes in accordance with an embodiment of the present disclosure
  • FIG. 3 illustrates a non-limiting flowchart example of a process for working the resinous mixture from FIG 1 in accordance with an embodiment of the present disclosure
  • FIG. 4 illustrates a non-limiting system implementing a process for making a hashish product in accordance with an embodiment of the present disclosure
  • FIG. 5 illustrates a non-limiting schematic of a setting for performing a gloss and reflectance measurement
  • FIG. 6A-6E are images of hashish product samples manufactured in accordance with Examples described herein;
  • FIG. 7 A is a comparative image comparing hashish product samples manufactured with a single-screw extruder (I) and a double-screw extruder (II); and
  • FIG. 7B is a comparative image comparing hashish product samples manufactured with pressing (I), single-screw extruder (II), and double-screw extruder (III).
  • the present inventors have developed a hashish product and industrial method of manufacturing same that addresses at least some of the above-identified problems.
  • the hashish product according to the present disclosure has a visual appearance that substantially matches the consumer appealing hand made products without systematic use of exogenous ingredients (such as coloring agents, oils, etc.) and/or additional post-manufacturing processing performed by the manufacturer or user to artificially impart such visual appearance.
  • the industrial hash of the present disclosure can be characterized with dark color and shiny appearance, as would be expected from a hand-rubbed hashish, or bubble hashish, or hash made with high potency kief.
  • the present inventors have developed an industrial manufacturing process to produce such hash product that includes mixing isolated cannabis trichomes under specific conditions that are sufficient to obtain a resinous mixture which upon retrieval through an extrusion die affords a hashish product having the desired appearance.
  • the process allows to have a shiny hash straight out of the die, without requiring further processing (e.g., rolling up as a ball, adding exogenous ingredients such as oils, etc.).
  • further processing e.g., rolling up as a ball, adding exogenous ingredients such as oils, etc.
  • Such difference also afforded a technical effect in that the resulting hash product can also be characterized as having a low moisture content, which can reduce or avoid likelihood of mold growth over time, thus affording advantageous extended shelf life to the hashish product compared to other industrial hashish with higher moisture content.
  • Such extended shelf life may also afford a technical effect in that this may avoid or minimize the need for irradiation (e.g., electron beams, x-rays or gamma rays).
  • irradiation e.g., electron beams, x-rays or gamma rays
  • irradiation is commonly used on food products to eliminate microorganism and thus extend shelf life
  • using irradiation on hashish products may be problematic for a number of reasons. For example, irradiation can be costly and time-consuming, especially multiple steps/doses of irradiation are implemented and/or if irradiation treatments are performed at an offsite location, which adds logistics to the overall costs.
  • the hashish product of the present disclosure comprises a cohesive mass of isolated cannabis trichomes.
  • the cohesive mass may be a substantially homogeneous cohesive mass of isolated trichomes.
  • substantially homogeneous it is meant that the hashish product has a constant or uniform distribution of isolated trichomes throughout its cohesive mass.
  • the manufacturing procedures described herein process the isolated trichomes in such fashion to result in mixing thereof into a substantially constant, uniform cohesive mass.
  • the term “cannabis trichomes” generally refers to crystal-shaped outgrowths or appendages (also called resin glands) on cannabis plants typically covering the leaves and buds. Trichomes produce hundreds of known cannabinoids, terpenes, and flavonoids that make cannabis strains potent, unique, and effective.
  • isolated cannabis trichomes refers to trichomes that have been separated from cannabis plant material using any method known in the art. The details of various methods for separating trichomes from the cannabis plant are well-known in the art. For example, and without wishing to be limiting in any manner, the isolated cannabis trichomes may be obtained by manual processes like dry sifting or by water extraction methods.
  • Solvent-less extraction methods can include mechanical separation of trichomes from the plant, such as sieving through a screen by hand or in motorized tumblers (see for example WO 2019/161509), or by submerging the cannabis plants in icy water (see for example US2020/0261824, which is herein incorporated by reference) and agitating to separate the trichomes from the plant and drying the trichomes. Because of inherent limitations to existing separation methods, some plant matter or other foreign matter can be present in isolated cannabis trichomes.
  • Isolated cannabis trichomes obtained by mechanical separation of trichomes from the cannabis plant biomass is typically referred to as “kief’ (also “keef” or “kif”) and has a powdery appearance. Typically, some residual plant material remains in the finished kief and thus in the resulting hashish product. In some embodiments, the isolated trichomes are dry-sift kief.
  • the isolated cannabis trichomes forming the hashish product of the present disclosure may originate from one or more than one strain of cannabis plant. It is known amongst consumers of hashish and other cannabis products that using isolated cannabis trichomes produced from more than one strain of cannabis plant allows a user to tune the psychoactive and/or entourage effect obtained by consuming the product.
  • the mixing of cannabis plant strains may also allow to adjust the final concentration of a component of the product, for example but not limited to the cannabinoid content. Additionally, use of more than one strain allows for improved product and waste management - important in commercial production.
  • hempbis generally refers to a genus of flowering plants that includes several species. The number of species is currently being disputed. There are three different species that have been recognized, namely Cannabis sativa, Cannabis indica and Cannabis ruderalis. Hemp, or industrial hemp, is a strain of the Cannabis sativa plant species that is grown specifically for the industrial uses of its derived products. In terms of cannabinoids content, hemp has lower concentrations of tetrahydrocannabinol (THC) and higher concentrations of cannabidiol (CBD), which decreases or eliminates the THC-associated psychoactive effects.
  • THC tetrahydrocannabinol
  • CBD cannabidiol
  • the hashish product of the present disclosure is characterized as having a desirable dark color, such as having a lightness value L* £ 50 on CIELAB scale.
  • assessing and/or measuring the color can be performed quantitatively using a colorimeter, a spectrophotometer, or qualitatively with the human eye.
  • the color can be measured by reflectance spectrophotometer ASTM standard test methodology.
  • Tristimulus L*, a*, b* values are measured from the viewing surface of the hashish product. These L*, a*, b* values are reported in terms of the CIE 1976 color coordinate standard (CIELAB scale).
  • the hashish product of the present disclosure has a lightness value L* £ 50 based on the CIELAB scale - e.g., the reader will readily recognize that such lightness value range leaves flexibility to the producer, as the product can be made darker through other means if desirable to favor consumer appeal.
  • the hashish product may have a lightness value L* from 0 to about 50 or any value therebetween, or in a range of values defined by any values therebetween.
  • the hashish product may have a lightness value L* up to about 50, up to about 45, up to about 40, up to about 35, up to about 30, up to about 25, up to about 20, up to about 15, up to about 10, up to about 5 or any value therebetween.
  • the hashish product may have a lightness value L* of from about 5 to about 45, of from about 10 to about 40, from about 15 to about 35, from about 20 to about 30.
  • the hashish product may have a lightness value L* of about 5, of about 10, of about 15, of about 20, of about 25, of about 30, of about 35, of about 40, of about 45, or about 50.
  • the hashish product of the present disclosure is characterized as having a desirable shininess, such as having a % reflectance of at least about 5%85.
  • reflectance is the proportional amount of reflected light measured from a sample surface, relative to the amount of reflected light measured from a reference plate and can thus serve to characterize the shininess of a hashish product.
  • %Reflectance can be determined in several ways all of which are known to the person skilled in the art. For example, %Reflectance could be determined by a glossmeter which initially determines shininess in terms of gloss by directing a constant intensity light beam, at a fixed angle Y, on to the test surface and monitoring the amount of reflected light from the same angle. The determined gloss value (also known as Gloss Unit or GU) is in turn translated to %reflectance. Whilst the Gloss Unit (GU) scale is linear, each angle of incidence has a different gloss measurement range; 0 - 2000 GU (for 20°), 0 - 1000 GU (for 60°) and 0 - 160 GU (for 85°).
  • %Reflectance compares the amount of light energy transmitted and received by a glossmeter and expresses the value as a percentage of the angle of incident's full measurement range and the value is displayed as a percentage relative to the selected angle of incidence. For example, as the measurement range for a 20° glossmeter is 0-2000 GU; a value of 1000 GU at 20° would be expressed in terms of %reflectance as 50%20, and a value of 500 GU would be expressed as 25%20. However, A value of 500 GU at 60°, but would be expressed as 50%60 as the measurement range for the 60° is 0 - 1000 GU.
  • gloss can be determined with the ElcometerTM 480 Model T glossmeter with integrated ElcoMasterTM software (Elcometer, USA).
  • Elcometer In order to determine the most appropriate measurement angle start with a gloss meter set at 60 degrees angle of incidence. If the result is between 10-70GU, the coating is termed ‘semi-gloss’ and should be measured using the 60 degrees angle. If the result is less than 10GU, the product is ‘low gloss’ and should be measured using the 85 degrees angle and if it is greater than 70GU, the product is known as ‘high gloss’ and should be measured using the 20 degrees angle.
  • the hashish product according to the present disclosure has a gloss value of at least 6 GU, at least 7 GU, at least 8 GU, or even greater (e.g., at least 9 GU, at least 10 GU, or more).
  • the hashish product according to the present disclosure has a %reflectance of at least 4%85, at least 4.5%85, at least 5%85, at least 5.5%85, or even greater (e.g., at least 6%85, at least 7%85, or more).
  • hashish shininess may depend on several factors, for example, the potency of the base materials, i.e.
  • the processing parameters to obtain the hash can affect the level of how much resin can be extracted from the trichomes, for example hand rubbing the hash may impart more mechanical / thermal energy to the kief thus extracting more resin therefrom compared to simply pressing the kief in an industrial press; post processing steps performed by the manufacturer and/or users, such as rolling the hashish product into a ball which has been reported to enhance the shiny aspect of hashish product that have sufficient resin content to expose at the outer surface of the hashish product; and the like.
  • a common trait being that higher potency / higher resin content correlates with better cohesion and smoothness as well as desired color and/or shininess. It was thus surprising to the inventors to be able to obtain hash with such desirable shininess without recourse to such procedures known to favor shininess. For example, the present inventors were able to obtain hand-rubbed hash shininess levels using dry-sift kief with an extruder device, where dry- sift kief is known to produce less shiny hash.
  • the resulting hash product can include a residual moisture content, which can originate for example from endogenous water present in the kief or other liquids, such as terpenes.
  • the hashish product of the present disclosure can comprise a moisture content of no more than about 8 wt.% (e.g., less than 8 wt.%), such as from about 2 wt.% to about 8 wt.% or any value therebetween, or in a range of values defined by any values therebetween.
  • the hashish product may have a moisture content of up to about 8 wt.%, of up to about 7 wt.%, of up to about 6 wt.%, of up to about 5 wt.%, of up to about 4 wt.%, of up to about 3 wt.%, or of up to about 2.5 wt.% or any value therebetween.
  • the hashish product may have a moisture content of from about 2.5 wt.% to about 4.5 wt.%, from about 2.8 wt.% to about 4.2 wt.%, from about 3.0 wt.% to about 4.0 wt.%, from about 3.2 wt.% to about 3.8 wt.%, or from about 3.4 wt.% to about 3.6 wt.%.
  • the present inventors measured an about 2.5 wt.% drop in moisture from processing the kief through the mixing process described herein to obtain a hash product having the desired characteristics (e.g., dark black, shiny, and malleable). For example, in a specific embodiment, the present inventors obtained a hash product having moisture content of 3-5 wt.% using a dry-sift kief having an initial moisture content of 7.4 wt.%.
  • water can be added into the process depending on specific applications.
  • water could be added to help more efficiently conduct thermal energy to the product and/or help form cohesive forces leading to a more malleable and soft texture.
  • water could be added in the form of liquid water, steam, or ice.
  • the water being added can be water purified using any known process, such as capacitive deionization, reverse osmosis, carbon filtering, microfiltration, ultrafiltration, ultraviolet oxidation, electrodeionization, distillation, and the like.
  • the moisture content of the hashish product can be determined by several methods known to the person skilled in the art including but not limited to Thermogravimetry Analysis (TGA) and equipment such as Mettler ToledoTM Hal. Moisture Analyzer HC103 (Fisher Scientific, USA) or MA160 Thermogravimetric Moisture Balance-type Analyzer (Sartorius Canada Inc).
  • TGA Thermogravimetry Analysis
  • MA160 Thermogravimetric Moisture Balance-type Analyzer Sudtorius Canada Inc.
  • the hashish product of the present disclosure comprises one or more cannabinoid(s).
  • the one or more cannabinoid(s) may be present endogenously in the isolated trichomes used to make the hash product or may be added in the form of an additional component (as described later in this text).
  • cannabinoid generally refers to any chemical compound that acts upon a cannabinoid receptor such as CBi and CB2.
  • cannabinoids include, but are not limited to, cannabichromanon (CBCN), cannabichromene (CBC), cannabichromevarin (CBCV), cannabicitran (CBT), cannabicyclol (CBL), cannabicyclovarin (CBLV), cannabidiol (CBD, defined below), cannabidiolic acid (CBDA), cannabidiol monomethylether (CBDM), cannabidiol- C4 (CBD-C4), cannabidiorcol (CBD-C1), cannabidiphorol (CBDP), cannabidivarin (CBDV), cannabielsoin (CBE), cannabifuran (CBF), cannabigerol (CBG), cannabigerol monomethylether (
  • Cannabidiol means one or more of the following compounds: A2-cannabidiol, D5- cannabidiol (2-(6-isopropenyl-3-methyl-5-cyclohexen-l-yl)-5-pentyl-l,3-benzenediol); D4- cannabidiol (2-(6-isopropenyl-3-methyl-4-cyclohexen-l-yl)-5-pentyl-l,3-benzenediol); D3- cannabidiol (2-(6-isopropenyl-3-methyl-3-cyclohexen-l-yl)-5-pentyl-l,3-benzenediol); D3,7- cannabidiol (2-(6-isopropenyl-3-methylenecyclohex-l-yl)-5-pentyl-l,3-benzenediol); D2- cannabidiol (2-(6-isopropenyl-3
  • Tetrahydrocannabinol means one or more of the following compounds: D8- tetrahydrocannabinol (Dd-THC), Dd-tetrahydrocannabivarin (Dd-THCV), A9-cis- tetrahydrocannabinol (cis-THC), A9-tetrahydrocannabinol (D9-THO), D10-tetrahydrocannabinol (DIO-THC), A9-tetrahydrocannabinol-C4 (THC-C4), A9-tetrahydrocannabinolic acid-C4 (THCA- C4), synhexyl (n-hexyl-A3THC).
  • THC means one or more of the following compounds: A9-tetrahydrocannabinol and D8- tetrahydrocannabinol.
  • the hashish product of the present disclosure contains the one or more cannabinoid(s) in an amount sufficient for the user to experience a desired effect when consuming the product.
  • the hashish product may comprise from about 5 wt.% to about 90 wt.% cannabinoid or any value therebetween, or in a range of values defined by any values therebetween.
  • the hashish product may comprise up to about 90 wt.%, up to about 80 wt.%, up to about 70 wt.%, up to about 60 wt.%, or up to about 50 wt.%, or up to about 40 wt.%, or up to about 30 wt.% or any value therebetween, or in a range of values defined by the aforementioned values.
  • the hashish product may comprise from about 10 wt.% to about 60 wt.%, more preferably from about 20 wt.% to about 50 wt.%.
  • the hashish product may include up to 1000 mg/g THC, depending on specific implementations of the present disclosure.
  • the hashish product of the present disclosure may include one or more cannabinoid, such as THC, CBD, CBG, CBN, or any combinations thereof.
  • THC can be delta-9-THC and/or delta-8-THC.
  • the cannabinoids can be in similar or different amounts, depending on specific implementations of the present disclosure.
  • a cannabinoid may be in an acid form or a non-acid form, the latter also being referred to as the decarboxylated form since the non-acid form can be generated by decarboxylating the acid form.
  • the content in the acid form and the decarboxylated form of a specific cannabinoid can be determined using suitable methods known to the person skilled in the art, such as but not limited to Gas Chromatography/ Mass Spectrometry (GC/MS), High Performance Liquid Chromatography (HPLC), Gas Chromatography/ Flame Ionization Detection (GC/FID), Fourier transform infrared (FT-IR) spectroscopy, and the like.
  • suitable methods are described, for example, in Formato et al. (-)-Cannabidiolic Acid, a Still Overlooked Bioactive Compound: An Introductory Review and Preliminary Research. Molecules. 2020 Jun 5;25(11):2638.
  • the hashish product according to the present disclosure may also comprise one or more additional components.
  • the one or more additional components may be added to alter the characteristics of the hashish product, such as cannabinoid content, potency, entourage effect, odor, color, shine, consistency, texture, malleability, and the like.
  • the one or more additional components may be substantially homogeneously distributed on at least a portion of a surface of the hashish product, for example as a coating, and/or the one or more additional components may be substantially homogeneously distributed throughout the cohesive mass forming the hash product.
  • the portion of the surface of the hashish product may include at least 20%, at least 30%, at least 40%, at least 50%, at least 60%, at least 70%, at least 80%, at least 90%, or 100% of the surface of the hashish product.
  • the one or more additional component may be any suitable food grade and/or non-toxic composition or component known in the art. As will be recognized by those of skill in the art, the toxicity of each type of additional component may be dependent on the method of consumption of the hashish product. For example, in applications where smoke / vapor produced by the hashish product is to be inhaled, suitable additional components may include, but are not limited to one or more cannabinoid, one or more terpene (also referred to herein as a “terpene blend”), water, one or more flavonoid, or any combination thereof.
  • the one or more additional component may be a cannabinoid.
  • the cannabinoid may be extracted from any suitable source material including, but not limited to, cannabis or hemp plant material (e.g., flowers, seeds, and trichomes) or may be manufactured artificially (for example cannabinoids produced in yeast, as described in WO WO2018/148848). Cannabinoids can be extracted from a cannabis or hemp plant material according to any procedure known in the art.
  • a “crude extract” containing a cannabinoid may be obtained by extraction from plant materials using for example aliphatic hydrocarbons (such as propane, butane), alcohols (such as ethanol), petroleum ether, naphtha, olive oil, carbon dioxide (including supercritical and subcritical CO2), chloroform, or any combinations thereof.
  • the crude extract may then be “winterized”, that is, extracted with an organic solvent (such as ethanol) to remove lipids and waxes (to produce a “winterized extract”), as described for example in US 7,700,368, US 2004/0049059, and US 2008/0167483, which are each herein incorporated by reference in their entirety.
  • the method for obtaining the cannabinoid may further include purification steps such as a distillation step to further purify, isolate or crystallize one or more cannabinoids, which is referred to in the art and herein as a “distillate”;
  • a distillation step to further purify, isolate or crystallize one or more cannabinoids
  • US20160346339 which is incorporated herein by reference, describes a process for extracting cannabinoids from cannabis plant material using solvent extraction followed by filtration, and evaporation of the solvent in a distiller to obtain a distillate.
  • the distillate may be cut with one or more terpenes.
  • the crude extract, the winterized extract or the distillate may be further purified, for example using chromatographic and other separation methods known in the art, to obtain an “isolate”.
  • Cannabinoid extracts may also be obtained using solvent-less extraction methods; for example, cannabis plant material may be subjected to heat and pressure to extract a resinous sap (“rosin”) containing cannabinoids; methods for obtaining rosin are well-known in the art.
  • the one or more additional component may thus include one or more cannabinoid in the form of a crude cannabis extract, a cannabis distillate, a cannabis isolate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
  • the one or more additional component may be a terpene.
  • terpene generally refers to a class of chemical components comprised of the fundamental building block of isoprene, which can be linked to form linear structures or rings. Terpenes may include hemiterpenes (single isoprenoid unit), monoterpenes (two units), sesquiterpenes (three units), diterpenes (four units), sesterterpenes (five units), triterpenes (six units), and so on. At least some terpenes are expected to interact with, and potentiate the activity of, cannabinoids. Any suitable terpene may be used in the hashish product of the present invention.
  • terpenes originating from cannabis plant may be used, including but not limited to aromadendrene, bergamottin, bergamotol, bisabolene, borneol, 4-3-carene, caryophyllene, cineole/eucalyptol, p-cymene, dihydroj asmone, elemene, farnesene, fenchol, geranylacetate, guaiol, humulene, isopulegol, limonene, linalool, menthone, menthol, menthofuran, myrcene, nerylacetate, neomenthylacetate, ocimene, perillylalcohol, phellandrene, pinene, pulegone, sabinene, terpinene, terpineol, 4-terpineol, terpinolene, and derivatives thereof.
  • terpenes include nerolidol, phytol, geraniol, alpha-bisabolol, thymol, genipin, astragaloside, asiaticoside, camphene, beta-amyrin, thujone, citronellol, 1,8-cineole, cycloartenol, hashishene, and derivatives thereof. Further examples of terpenes are discussed in US Patent Application Pub. No. US2016/0250270, which is herein incorporated by reference in its entirety for all purposes.
  • the hashish product of the present disclosure may contain one or more terpene(s).
  • the one or more terpene(s) may originate from the hashish, from an additional component, or both.
  • the hashish product of the present disclosure may include the one or more terpene(s) in an amount (the “terpene content”) sufficient for the user to experience a desired entourage effect when consuming the product.
  • the hashish product may comprise from about 0.5 wt.% to about 15 wt.% terpene, for example up to about 15 wt.%, or up to about 10 wt.%, or up to about 5 wt.%, or up to about 4 wt.%, or up to about 3 wt.%, or up to about 2 wt.%, or up to about 1 wt.%.
  • the one or more terpene(s) may include hashishene.
  • hashishene is believed to be a terpene produced by rearrangement of myrcene that may be found in hashish after mechanical processing, and that may be responsible for the typical desirable “hashish flavour”.
  • the one or more additional component may be a flavonoid.
  • flavonoid refers to a group of phytonutrients comprising a polyphenolic structure. Flavonoids are found in diverse types of plants and are responsible for a wide range of functions, including imparting pigment to petals, leaves, and fruit. Any suitable flavonoid may be used in the hashish product of the present invention.
  • flavonoids originating from a cannabis plant may be used, including but not limited to: apigenin, cannflavin A, cannflavin B, cannflavin C, chrysoeril, cosmosiin, flavocannabiside, homoorientin, kaempferol, luteolin, myricetin, orientin, quercetin, vitexin, and isovitexin.
  • the one or more additional component may include a combination of any one of the one or more additional component described herein.
  • hashish is typically used for recreational or medicinal uses.
  • hashish products can be used to achieve a desired effect in a user, such as a psychoactive effect, a physiological effect, or a treatment of a condition.
  • psychoactive effect it is meant a substantial effect on mood, perception, consciousness, cognition, or behavior of a subject resulting from changes in the normal functioning of the nervous system.
  • physiological effect it is meant an effect associated with a feeling of physical and/or emotional satisfaction.
  • treatment of a condition it is meant the treatment or alleviation of a disease or condition by absorption of cannabinoid(s) at sufficient amounts to mediate the therapeutic effects.
  • treating is used herein to mean obtaining a desired pharmacologic and/or physiologic effect.
  • the effect may be prophylactic, in terms of completely or partially preventing a disease, condition, or symptoms thereof, and/or may be therapeutic in terms of a partial or complete cure for a disease or condition and/or adverse effect, such as a symptom, attributable to the disease or disorder.
  • Treatment covers any treatment of a disease or condition of a mammal, such as a dog, cat or human, preferably a human.
  • the disease or condition is selected from the group consisting of pain, anxiety, an inflammatory disorder, a neurological disorder, a psychiatric disorder, a malignancy, an immune disorder, a metabolic disorder, a nutritional deficiency, an infectious disease, a gastrointestinal disorder, and a cardiovascular disorder.
  • the disease or condition is pain.
  • the disease or condition is associated with the feeling of physical and/or emotional satisfaction.
  • the “effective amount” administered and rate and time- course of administration will depend on the desired effect associated with a feeling of physical and/or emotional satisfaction in the subject.
  • the “effective amount” administered, and rate and time-course of administration will depend on the nature and severity of the disease or condition being treated and typically also takes into consideration the condition of the individual subject, the method of administration and the like.
  • the hashish product may be produced by mixing the components thoroughly to provide a resinous mixture having desired characteristics.
  • the mixing may be performed by mechanically mixing.
  • mechanically mixing or “mechanical mixing”, it is meant mixing using any suitable mechanical means.
  • the mechanical means may be, for example, a plurality of interpenetrate helicoidal surfaces within an elongated enclosure or barrel, a non-limiting example of which is an extruder apparatus.
  • An extruder apparatus is a machine used to perform an extrusion process. Manufacturing by extrusion occurs when a material (usually pellets, dry powder, rubber, plastic, metal bar stock or food) is heated and pushed through a die assembly.
  • a die is a mold that shapes the heated material as it is forced through a small opening from the inside of the extruder to the outside.
  • the extruder can mix the ingredients, and optionally adding heating, while propelling the extrudate through the die, for example to impart a desired shape to the hashish product.
  • Extruders use in the industry are often of single-screw or twin-screw type.
  • Twin-screw extruders are known in the art - screws of such extruders may be parallel or non-parallel, converging or non-converging, with or without differential speed, counter or non counter rotating as described for example in US 6,609,819, WO 2020/220390, WO 2020/220495 and US 2010/0143523, where each of which is herein incorporated by reference in its entirety. It will be readily appreciated that extruders have flexible configuration (in terms of mixing zones, temperature zones, input zones, etc.) and that any suitable configuration of an extruder apparatus capable of producing a hashish product may be used within the context of the present disclosure.
  • a twin-screw extruder can be configured to have one or more mixing zones, one or more conveying zones, or one or more compression zones. Each of the zones may have input ports used for introduction of material. The mixing zones apply shear forces to the input materials, blending until they are homogenized.
  • the extruder die assembly may perform a variety of functions: it may form or shape the extrudate, it may divide the extrudate into multiple extrudates, it may inject one or more component into the extrudate, and it may compress and reduce the cross-sectional area of the extrudate.
  • extruders have flexible configuration (in terms of mixing zones, conveying zones, compression zones, etc.) and that any suitable configuration of an extruder apparatus (with any axial temperature profile or with any number of input ports) capable of producing a hashish product may be used within the context of the present disclosure.
  • such high heat and shear can be created from mechanical mixing elements such as mixing pins and/or reverse flow elements.
  • the reverse flow elements can increase the retention time of material on the mixing elements that it precedes.
  • the mixing pins and reverse flow elements collectively can result in a tightly packed area that contributes to an increase in heat transfer efficiency. Such configurations can thus afford darker and shinier hashish product compared to hashish product manufactured with industrial press or single screw extruder.
  • FIG. 1 is a non-limiting flowchart of a process 100 for making a hashish product in accordance with an embodiment of the present disclosure.
  • the process 100 comprises a first step 110 of providing isolated cannabis trichomes.
  • the isolated cannabis trichomes may include trichomes isolated from a single cannabis strain.
  • the isolated cannabis trichomes may include trichomes isolated from a plurality of distinct cannabis strains, which may have different respective cannabinoid(s) and/or terpene(s) content.
  • the choice of one over the other may be driven by practical considerations, such as but not limited to inventory management considerations, the desired cannabinoid content of the hashish product, the desired user experience, and the like. It is known amongst consumers of hashish and other cannabis products that using isolated cannabis trichomes produced from more than one strain of cannabis plant may allow a user to tune the psychoactive, medical and/or entourage effect obtained by consuming the product. The mixing of cannabis plant strains may also allow adjustments to the final concentration of a component of the product, for example but not limited to the cannabinoid content. Additionally, use of more than one strain allows for improved product and waste management - important in commercial production.
  • the isolated cannabis trichomes may be obtained in several ways.
  • the producer implementing the process 100 may obtain the isolated cannabis trichomes from another producer.
  • the step 110 may thus include a sub-step of obtaining the isolated cannabis trichomes from another producer (not shown in figures).
  • the producer implementing the process 100 may obtain the isolated cannabis trichomes via the following variants of step 110.
  • FIG. 2 is a variant 110’ which includes starting from cannabis plant material to isolate the cannabis trichomes therefrom.
  • a first step 210 includes providing cannabis plant material comprising cannabis trichomes.
  • the cannabis plant material may comprise cannabis flowers / buds, cannabis trim, cannabis leaves, or any combination thereof.
  • the producer implementing the first variant step 110’ may also produce the cannabis plant material or may obtain the cannabis plant material from another producer.
  • a second step 220 cannabis trichomes are isolated therefrom, thus resulting in the isolated cannabis trichomes.
  • various processes for isolating cannabis trichomes from cannabis plant material are known and as such, will not be further described here.
  • the variant step 110’ may be performed at a first location while the remaining steps of process 100 may be performed at a second location, where the first and second locations may be within the same licensed producer site or within different licensed producer sites. In some embodiments, all steps of process 100 may be performed at the same location.
  • the process 100 further comprises a step 130 of mixing the isolated cannabis trichomes.
  • the mixing includes applying compression and shear forces to the isolated cannabis trichomes via a plurality of interpenetrate helicoidal surfaces within an elongated enclosure.
  • the elongated enclosure is an extruder device having at least two screws.
  • the isolated cannabis trichomes are mixed while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture.
  • the resinous mixture is a substantially homogeneous mixture.
  • the conditions to form the resinous mixture at the mixing step 130 comprise shear, pressure, and temperature, which may be varied to alter the characteristics of the hashish product.
  • characteristics may include, but without being limited to homogeneity, lightness, %reflectance, stiffness (i.e. , characteristic that defines the level of malleability of the hashish product), hardness or resistance to localized deformation (i.e., characteristic that determines how easy it is to cut or separate the hashish product), toughness (i.e., characteristic that determines the likelihood that the hashish product deforms rather than fractures under an applied force), color, tactual characteristics, and the like.
  • the pressure being applied at the mixing step 130 may be at a value of about 1 bar or more.
  • a pressure of from about 1 bar to about 70 bar including any ranges therein or any value therein.
  • a given pressure value may be selected depending on the die that is used to form the hashish product, as described elsewhere in this text.
  • the temperature being applied at the mixing step 130 may be at a value of about 170°C or less.
  • different temperatures corresponding to the abovementioned temperature values or ranges may be used in different zones during the process as described elsewhere in this text.
  • the mixing shear and compressive forces can be controlled by modulating the rotational speed of the screws within the extruder.
  • the extruder screws rotation per minute (rpm) can be selected to perform the mixing step 130 at a value of for example about 10 rpm or more.
  • extruder screws rpm can be selected in a range of from about 10 rpm to about 1000 rpm, including any ranges therein or any value therein. For example, from about 15 to about 500 rpm, or from about 25 to about 450 rpm, or from about 30 to about 400 rpm, or from about 45 to about 450 rpm including any value within any of these ranges and preferably between 100 rpm and 200 rpm.
  • the residence time within the extruder barrel can be directly related to the length of the barrel and the rotational speed of the twin screws.
  • the components can travel through at least one zone of the barrel in a distal direction, and then be redirected to at least one zone of the barrel in a proximal direction (i.e., towards the inlet rather than towards the die).
  • Optional step 120 includes incorporating one or more additional component at one or more steps during the process 100.
  • one or more additional component can be added to the isolated trichomes prior to, simultaneously with, or following step 110, or prior to, simultaneously with, or following the mixing step 130. Multiple additional components may be added in a single step or may be added separately in one or more consecutive steps or at different times or points along the process 100.
  • the one or more additional components can be one or more cannabinoids, one or more terpenes, one or more flavonoids, one or more flavoring agents, one or more non-toxic coloring agents, or any combination thereof.
  • the cannabinoid may be provided in the form of a cannabis extract (including a crude extract, or a winterized extract), a distillate, an isolate, cannabis rosin, cannabis resin, cannabis wax, or cannabis shatter.
  • the one or more additional component may be incorporated during the process (through one or more input ports located at each of the zones within the extruder length, as described elsewhere in this text) to produce the hashish product.
  • the one or more additional component may be substantially homogeneously distributed throughout the hashish product.
  • step 130 At least a portion of the resinous mixture is retrieved at step 140 to obtain an individual unit of hashish product having a cohesive mass of the isolated trichomes.
  • the hashish product may have a substantially homogeneous cohesive mass of the isolated trichomes.
  • FIG. 3 includes additional steps that can follow step 140 of the process 100 in FIG. 1.
  • the at least portion of the resinous mixture can be passed through a die at step 150, which may be configured to impart a pre-determined shape thereto.
  • the at least portion of the resinous mixture may be cooled at step 145.
  • the solid or semi-solid hashish product from step 150 may optionally further undergo post processing steps.
  • the solid or semi-solid hashish product from step 150 may be cut to a pre-determined cutting pattern, a pre-determined weight, or a pre-determined length to obtain smaller units of hashish product for a pre-determined packaging size (not shown in the figures).
  • FIG. 4 illustrates a system 400 for implementing the process 100 to make a coherent and cohesive mass 480 in accordance with an embodiment.
  • the system 400 includes an extruder apparatus 410 that uses mechanical mixing means to amalgamate the isolated cannabis trichomes 420 into the coherent and cohesive mass 480.
  • the system 400 comprises a feed hopper 425 through which the isolated cannabis trichomes 420 are fed.
  • one or more additional component(s) 440 are fed through the feed hopper 425 and/or through one or more input port 445 located along the length of the apparatus 410 at locations corresponding to one or more predetermined portions or zones 450A-G of the extruder apparatus 410.
  • non-limiting examples of such one or more additional component(s) 440 include, for example, terpenes, flavonoids, cannabinoids in the form of crude extracts, distillates, isolates, winterized cannabis extracts, rosin, shatter, or resins, or any combinations thereof.
  • the extruder apparatus 410 is powered by a motor (not shown) that drives at least two extruder screws 430 to apply pressure and mechanical shear on the isolated cannabis trichomes 420 and optionally the one or more additional component(s) 440 entering the extruder 410 (for the sake of brevity only one screw of the twin-screw is illustrated in Fig. 4).
  • the extruder screws 430 may be configured for applying compression and shear forces to the isolated cannabis trichomes 420 via a plurality of interpenetrate helicoidal surfaces present along at least a portion of the extruder screws 430.
  • the extruder apparatus 410 may also implement a pressure sensing element 460 at the die vicinity zone 455 which is a measure of the shear force applied on the isolated cannabis trichomes 420 packing them into a cohesive mass.
  • the pressure may be at a value of about 1 bar or more. For example, a pressure of from about 1 bar to about 70 bar, including any ranges therein or any value therein.
  • a pressure of from about 1 bar to about 65 bar, from about 3 bar to about 60 bar, from about 4 bar to about 55 bar, from about 6 bar to about 50 bar, from about 8 bar to about 45 bar, from about 10 bar to about 40 bar, from about 12 bar to about 35 bar, from about 12 bar to about 32 bar, from about 14 bar to about 30 bar, from about 16 bar to about 28 bar, from about 18 bar to about 26 bar, or from about 20 bar to about 24 bar including any ranges therein or any value therein.
  • the system 400 may also implement heating by maintaining a set of predetermined temperature within the one or more predetermined portions or zones 450A-G of the extruder apparatus 410, or throughout the length of the extruder apparatus 410, depending on specifics applications.
  • the temperature being applied within each of the one or more predetermined portions or zones 450A-G of the extruder apparatus 410 may be at a value of about 170°C or less, the temperature in one zone being selected independently from another.
  • each of the one or more predetermined portions or zones 450A-G can independently be at a temperature selected within the range of from about 20°C to about 170°C, including any ranges therein or any value therein.
  • each of the one or more predetermined portions or zones 450A-G can independently be at a temperature of about 20°C, about 25°C, about 30°C, about 35°C, about 40°C, about 45°C, about 50°C, about 55°C, about 60°C, about 65°C, about 70°C, about 80°C, about 90°C, about 100°C, about 110°C, about 120°C, about 130°C, about 140°C, about 150°C, about 160°C, or about 170°C.
  • heating is also implemented at the extruder die by maintaining a predetermined temperature at the die zone 455.
  • the system 400 may also implement several zones across the length of the apparatus 410 each performing a single functionality including but not limiting to conveying, mixing, compressing, and reversing the flow direction of the resinous mixture (or isolated cannabis trichomes).
  • the operating parameters of the extruder apparatus 410 such as those discussed previously (e.g., temperature, pressure, and extruder screws rpm), can be selected to alter residence time of the resinous mixture (or isolated cannabis trichomes 420) in the extruder apparatus 410 to obtain the cohesive mass 480.
  • operating parameters such as heat and extrusion speed change the pressure experienced at the die and may alter the characteristics of the hashish product discussed above.
  • the pressure applied by the extruder screws can be accompanied by different temperature settings within each portions or zones 450A-G of the extruder to enhance mixing of the isolated cannabis trichomes, extract the resinous content of the trichomes and obtain a heated, cohesive, continuous, resinous mixture, preferably substantially homogenous resinous mixture.
  • the heating and mixing can continue until a desired level of homogeneity is obtained.
  • the heating may additionally advantageously assist in mixing the isolated cannabis trichomes 420 and optional additional components 440 to form the cohesive mass 480.
  • the heating can assist in at least partially melting optional additional components 440, such as cannabinoid isolate.
  • the heat may be applied through heating elements (not shown) embedded with the extruder screws 430 extending along the one or more predetermined portions or zones 450A-G across the length of the extruder 410.
  • heating elements not shown
  • one or more temperature controlling units can also be associated with the extruder apparatus 410 to monitor heat within the certain zone 450A-G of the extruder apparatus 410 and take any necessary action in the event of major deviations from the intended extrusion temperature.
  • At least a portion of the resinous mixture exits an extruder die 470 at the outlet of the extruder apparatus 410 in the form of an elongated, continuous solid or semi-solid cohesive mass 480.
  • the die 470 may impart any pre-determined shape to the cohesive mass 480.
  • the long and continuous solid or semi-solid cohesive mass 480 can be subjected to ambient temperature and pressure.
  • a cutting means 485 may be placed downstream of the extruder die 470 to cut the cohesive mass 480 according to a pre-established cutting pattern.
  • the pre-established cutting pattern may comprise cutting the cohesive mass 480 along a transverse axis and at pre-determined time intervals to obtain hashish product units of a pre-determined length and/or weight.
  • the cutting means can act intermittently to cut the cohesive mass 480 into individual units of hashish product 510.
  • the individual units of hashish product could be further transferred onto a flat conveyor belt or fall under gravity over an inclined conveyor belt (not shown) and sent for packaging and/or storage.
  • FIG. 5 illustrates a non-limiting schematic of a system 500 for determining gloss and %reflectance of the hashish product 520 using a glossmeter 510.
  • the hashish product 510 may lie on a flat surface and the glossmeter 510 is placed on top of the hashish product.
  • the glossmeter 510 has a built-in light emitter 530A that directs incident light 540A onto the surface of the hashish product with an incidence angle Y.
  • Reflected light 540B is the light reflected from the surface of the hashish product at the same angle as the incident angle Y and is sensed by a built-in photodetector 530B.
  • Diffuse reflected lights 550 are lights reflected in all directions with angles 1Y.
  • hashish products having a moisture content above 8 wt.% relative to total weight of the hashish product increased the likelihood of mold formation within 1-2 weeks.
  • hashish products made according to principles described herein are discussed below.
  • a sample of the hashish product was prepared and tested to measure various characteristics of the hashish product, such as %reflectance, etc.
  • the sample was prepared by flattening a portion of the hashish product for 30 seconds at a pressure of 9000 psi on a 3 in. x 5 in. area die.
  • the %reflectance of the hashish product was determined by measuring gloss units (GU) using a LANDTEK GM-268 glossmeter set up with an 85° angle of incidence.
  • a batch of isolated cannabis trichomes was loaded into the feed hopper (zone 1) of a Pharma 11 twin-screw extruder (ThermoFisher ScientificTM, USA) with parallel 11mm diameter twin screws and length-to-diameter ratio (L/D) of 40:1 segmented into 7 processing zones (zone 2 to zone 8).
  • a chiller circulating water at 10°C was used to implement temperature control within the processing zones as well as the die.
  • the initial extruder setup (I) featured two mixing zones (“MIX”) within the middle part of the extruder (i.e. , zones 4 and 6) and a compression zone (“COMP”) at the end of the screw (zone 8), as set forth in Table EX-1-1 :
  • the isolated cannabis trichomes were fed in the twin-screw extruder with a feed rate of 1.7 g/min.
  • the twin-screw extruder having a torque of 5-8%, an rpm of 300 and a 7mm die (pressure of 0-1 bar, temperature 70°C or 90°C).
  • the temperature profile across the extruder length was according to Table EX- 1-2:
  • extruder setup (I) from Example 1 was maintained while a die with smaller diameter (4.5 mm) was employed resulting in an increase in cohesiveness and darker color of the extruded hashish product.
  • extruder setup (I) from Example 1 and die diameter of Example 2 (4.5 mm) were maintained while the extruder feed was 94 wt.% isolated cannabis trichomes and 4% water to further assist flow through the extruder. Also, the temperature at the die and within the mixing zones were lowered to lessen the separation of resin from the trichomes.
  • Isolated cannabis trichomes (Meridian strain) with a feed rate of 2.5 g/min (94 wt% isolated cannabis trichomes and 4% water) were fed to the twin-screw extruder at an rpm of 300, a 10% torque, die temperature and pressure of 80°C and 1 bar, respectively.
  • the temperature profile across the extruder length was according to Table EX-3-1:
  • Example 3 identical process parameters as those of Example 3 were implemented except that water was not added in the feed stream. Also, to analyze the effects of torque, die temperature, die pressure and temperature across extruder zones on the hashish product, these conditions were also varied in this example. [0140] Isolated cannabis trichomes (Meridian strain) with a feed rate of 2.5 g/min were fed to the twin-screw extruder at a reduced rpm of 100 and under the following conditions as set forth in Tables EX-4-1 to EX-4-3:
  • extruder setup (I) from Example 1 was maintained. However, in order to achieve a shiny hashish product, it was postulated to increase the mechanical work by decreasing the die diameter to 2 mm thus generating more pressure. Also, to analyze the effects of extruder rpm and zone temperatures on the hashish product, these conditions were varied in this example.
  • the hashish products were kept in sealed ZiplocTM bags, placed in a plastic container, at room temperature with exposure to daylight.
  • the hashish products corresponding to EX- 5-1 to EX-5-3 had reflectance values of 6.8 GU, 6.9 GU and 7.3 GU, respectively, corresponding to %reflectance values of 4.2%85, 4.3%85 and 4.6%85, respectively.
  • Extruder setup (II) distinguishes from extruder setup (I) in the presence of a reverse flow segment (“REV”) after the first mixing zone with the aim of increasing retention time of isolated cannabis trichomes in the mixing zone (more mechanical and thermal energy transfer).
  • REV reverse flow segment
  • the overall breakdown for the extruder setup (II) is set forth in Table EX-6-1 :
  • Table EX-6-1 Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2.5 g/min were fed to the twin-screw extruder and under the following conditions as set forth in Tables EX-6-2 to EX-6-5 to assess the impact of change in screw step and temperature variation at the die and within different zones:
  • Table EX-6-5 [0158] It was observed from operating conditions I) to IV) that the obtained hashish products were darker in color and more malleable compared to those obtained in Examples 1 to 5 that employed the initial screw setup (I) without a reverse flow element. Further, comparing the hashish products obtained across operating conditions I) to IV) of this Example, the surface of the hashish product from operating condition IV) was less smooth and less shiny compared to that of operating condition III). Hashish product obtained from operating condition III) was the only one exhibiting shiny characteristic. The overall improvement in product characteristics in this Example compared to previous Examples was attributed to increased residence time (due to addition of reverse flow element).
  • Extruder setup (III) distinguishes from extruder setup (II) in the presence of a second compression element after the lead element while the two mixing sections were combined upstream of the reverse flow element.
  • the mixing section was placed near the compression elements, spanning the last two heated zones as set forth in Table EX-7-1 : Table EX-7-1
  • Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min were fed to the twin-screw extruder and under the following conditions as set forth in Tables EX-7-2 to EX-7-5 to assess the impact of change in screw step and temperature variation at the die and within variable zones:
  • the preferred temperature range was from about 100°C to about 120°C. It is hypothesized that the product could be made further soft and malleable by increasing the shear forces experienced by the product via the elongation of compression and mixing segments or via an increase in retention time within the mixing segments. Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed ZiplocTM bags, placed in a plastic container, at room temperature with exposure to daylight.
  • the hashish products corresponding to EX-7-2 to EX-7-5 had reflectance values of 6.9 GU, 7.1 GU, 7.3 GU and 7.1 GU, respectively, corresponding to %reflectance values of 4.3%85, 4.4%85, 4.5%85 and 4.4%85, respectively.
  • hashish product infused with CBD was manufactured using the extruder set up (II) as set forth in Table EX-8-1.
  • Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min were fed to the twin-screw extruder.
  • CBD distillate was introduced via a liquid feeding port in zone 3 through use of a syringe that dispensed the molten product at 60°C at a programmed feed rate.
  • the extruder was operated with the following operating conditions as set forth in Tables EX-8-2, EX-8-4 and EX-8-6:
  • the hashish products were kept in sealed ZiplocTM bags, placed in a plastic container, at room temperature with exposure to daylight.
  • the hashish products corresponding to EX-8-2 and EX-8-4 had reflectance values of 7.5 GU and 7.7 GU, respectively, corresponding to %reflectance values of 4.6%85 and 4.8%85, respectively.
  • hashish product infused with CBD isolate was manufactured in order to compare the resulting hashish product characteristics with that of Example 8. Same extruder setup (II) as that one of Example 8 was used.
  • Isolated cannabis trichomes (NLxBB strain) and CBD isolate were mixed using a commercially available KitchenAidTM mixer and the mixture was fed to the twin-screw extruder at a rate of 2 g/min and under the following operating conditions as set forth in Tables EX- 9-1 to EX- 9-2: [0176] Operating condition I): control with no CBD isolate infusion
  • Table EX-9-3 [0179] It was visually observed that the addition of CBD isolate to isolated cannabis trichomes and feeding them as a mixture to the twin-screw extruder resulted in a lower torque and die pressure as the CBD isolate melted during extrusion and seemingly provided lubrication to the extruding material. Like Example 8, the resulting hashish product upon addition of CBD isolate was a shinier, softer and more malleable hashish product compared to the control hashish product obtained from operating condition I). Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed ZiplocTM bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish products corresponding to EX-9-1 and EX-9-2 had reflectance values of 7.4 GU and 7.9 GU, respectively, corresponding to %reflectance values of 4.6%85 and 4.9%85, respectively.
  • Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min were fed to the twin-screw extruder.
  • CBD distillate was introduced via a liquid feeding port in zone 3 through use of a syringe that dispensed the molten product at 60°C at a programmed feed rate.
  • the extruder was operated with the following operating conditions as set forth in Tables EX-10-1, EX-10-3, EX- 10-5 and EX- 10-6:
  • the hashish products were kept in sealed ZiplocTM bags, placed in a plastic container, at room temperature with exposure to daylight.
  • the hashish products corresponding to EX-10-1, EX-10-3, EX-10-5 and EX-10-6 had reflectance values of 7.4 GU, 7.9 GU, 8.8 GU and 8.9 GU, respectively, corresponding to %reflectance values of 4.6%85, 4.9%85, 5.5%85 and 5.6%85, respectively.
  • the present inventor believes that there is a change in product flow through the die upon increase in distillate feeding as the product softens and that the hashish product needs to exit the die at a cooler temperature in order to remain smooth
  • Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min were fed to the twin-screw extruder.
  • CBD distillate was introduced via a liquid feeding port in zone 3 through use of a syringe that dispensed the molten product at 60°C at a programmed feed rate.
  • the extruder was operated with the following operating conditions as set forth in Tables EX-11-1 to EX-11-3:
  • control hashish products (operating condition I)) were malleable and had a shiny black and smooth appearance. However, they were tougher compared to the hashish product from operating condition II) which were in turn tougher than those obtained from operating condition III). In fact, hashish products obtained under operating condition III) was less smooth as it was becoming increasingly soft due to increase in distillate feed rate. The appearance characteristics are shown in FIG. 6E (corresponding to operating conditions I) to III)). Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed ZiplocTM bags, placed in a plastic container, at room temperature with exposure to daylight.
  • the hashish products corresponding to EX-11-1 , EX-11-2 and EX-11-3 had reflectance values of 7.3 GU, 8.7 GU and 8.7 GU, respectively, corresponding to %reflectance values of 4.5%85, 5.4%85 and 5.4%85, respectively.
  • hashish products are manufactured using a kief batch from Meridian strain by three distinct methods of extrusion with a twin-screw extruder (Pharma 11 twin-screw extruder (ThermoFisher ScientificTM, USA), extrusion with single-screw extruder (ETPI Lab extruder - Bonnot Company, USA as described for example in PCT/CA2021/050673) and pressing with an industrial press (for example as described in PCT/CA2020/051733).
  • the following operating conditions were used in each case, as set forth in Table EX-12-1.
  • Table EX- 12-1 Table EX- 12-1
  • High potency kief can make shiny hash more easily than low potency hash as it is easier bring out the resin to the surface.
  • Hash that has been post-processed to impart better surface uniformity, such as when rolling into a ball, will also make any hash shinier.
  • Higher potency can be obtained when making hash from trichomes isolated with water and ice methods (i.e., “bubble hash”), which have less impurities and higher potency. Dry sift kief, in contrast, necessitates a lot of mechanical and/or thermal energy to get that shine / gloss.
  • the present inventors have demonstrated that with the process described herein, which preferably uses a twin-screw extruder, there is sufficient energy input when mixing any type of kief, such as low potency, dry sift kief, etc., to facilitate resin oozing out from the trichomes and imparting better characteristics to the hashish product.
  • any type of kief such as low potency, dry sift kief, etc.
  • the terms “around”, “about” or “approximately” shall generally mean within the error margin generally accepted in the art, such as for example +/- 20%, +/- 15%, +/- 10%, or +/- 5%.
  • numerical quantities given herein generally include such error margin such that the terms “around”, “about” or “approximately” can be inferred if not expressly stated.
  • concentration and “content” are used interchangeably and refer to the weight or mass fraction of a constituent, i.e., the weight or mass of a constituent divided by the total mass of all constituents, and is expressed in wt.%, unless stated otherwise.

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Abstract

The present disclosure relates to industrial hashish products and industrial process for manufacturing same. The process comprises mixing isolated cannabis trichomes while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture and retrieving at least a portion of the resinous mixture through an extrusion die to obtain the hashish product. The hashish product is characterized as having a substantially homogeneous cohesive mass of the isolated trichomes that may have a % reflectance of at least 4%85, which substantially matches consumer appealing hand-made products, may have a moisture content of no more than about 8 wt.%, and/or may be free of exogenous water. The process is capable of automation and does not require use of coloring agents or post-processing steps to artificially impart desired visual characteristics that are typically associated with good quality hashish.

Description

INDUSTRIAL HASHISH AND METHOD FOR PRODUCING SAME AT AN INDUSTRIAL
SCALE
CROSS REFERENCE TO RELATED APPLICATION
[0001] The present application claims the benefit of U.S. provisional patent applications serial number 63/183,385, 63/185,210 and 63/278,916 filed respectively on May 3, 2021, May 6, 2021, and November 12, 2021. The contents of the above-referenced documents are incorporated herein by reference in their entirety.
TECHNICAL FIELD
[0002] This application generally relates to the field of industrial hashish products and methods of manufacturing hashish products at an industrial scale.
BACKGROUND
[0003] Hashish (or hash) is a concentrated derivative of cannabis plants, the dried resin glands of the flowering tops of mature and unpollinated female cannabis plants. The resin glands are known as trichomes. It contains the same active ingredients as the cannabis plants - including cannabinoids - yet at higher concentration levels than the un-sifted buds or leaves from which dried marijuana is made, which is tantamount to higher potency.
[0004] The cannabis trichomes are substantially isolated from cannabis plant matter. The isolated cannabis trichomes are usually collected by hand, by mechanical beating of the cannabis plants or by submersing the cannabis plants in icy water and then using small sieves to isolate the cannabis trichomes. Alternatively, mechanical isolation may be used to isolate cannabis trichomes from cannabis plant matter, such as sieving through a screen by hand (i.e. , dry sift) or in motorized tumblers, as described for example in WO 2019/161509. Isolated cannabis trichomes have a powder appearance (typically referred to as “kief”) and are pressed to obtain blocks of hashish.
[0005] The production of hashish is very labor intensive, and it is practically an art, where the skills of the individual play a key role in defining the quality and/or physical characteristics of the finished hashish product. The consistency and appearance of hashish vary depending on the manufacturing process and amount of leftover plant material (e.g., chlorophyll). Consumers often associate the hash color or smell to quality and/or origin. [0006] Good-quality pressed dry-sift hashish ranges in appearance from light blondish-brown, to greenish or dark-brown. Examples thereof include “Lebanese” hashish, which is from yellow to reddish, and “Moroccan” hashish which is from greenish to darker brown.
[0007] Hand-rubbed pressed hashish is most commonly referred to as being “Afghani” (from Afghanistan) or “Charas” (from India and Pakistan). This form of hashish is produced by rubbing the living plants to remove the sticky resin, which is then rolled into balls or eggs and left to cure before being consumed or sold. Hand-rubbed types of hash should be smooth, black or brownish- black, and often sticky to the touch. When opened, consumers expect the interior to be a delicate brown, perhaps with a slight green tinge (a very green interior indicates excessive residual plant material).
[0008] Current industrial hashish production requires multiple steps and often lack automation. For example, it has been reported that some companies employ several individuals to produce hand-rubbed hashish, which is not easily scaled and very costly for commercial production. Industrial presses have been reported for producing pressed dry-sift hashish, but difficulties in matching the traditionally hand-made hashish products in terms of appearance, malleability and more specifically color and shininess, have rendered this approach less appealable to the industry. The current methods for manufacturing hash at an industrial scale thus remain unsatisfactory.
[0009] Considering the above, it would be highly desirable to be provided with an industrial hashish product and manufacturing method for making same that would at least partially alleviate the disadvantages of the existing technologies.
SUMMARY
[0010] This Summary is provided to introduce a selection of concepts in a simplified form that are further described below in the Detailed Description. This Summary is not intended to identify key aspects or essential aspects of the claimed subject matter.
[0011] The present inventors have developed a hashish that matches the consumer appealing hand-made products where the manufacturing method can be at least partially automated and which does not require use of coloring agents or post-processing steps to artificially impart desired visual characteristics that are typically associated with good quality hashish. [0012] In a broad aspect, the present disclosure relates to a process of making a hashish product, comprising providing isolated cannabis trichomes; mixing the isolated cannabis trichomes while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture; and retrieving at least a portion of the resinous mixture through an extrusion die to obtain the hashish product, wherein the hashish product is a substantially homogeneous cohesive mass of the isolated trichomes having a % reflectance of at least 4%85.
[0013] In specific embodiments, the process may include one or more of the following features:
• the hashish product has a lightness value L* £ 50 on CIELAB scale, preferably from 0 to about 40, or of from about 10 to about 30, or of from about 15 to about 25.
• the hashish product has a % reflectance of at least 4.5%85, at least 5%85, or at least 5.5%85.
• the mixing includes applying compression and shear forces to the isolated trichomes via a plurality of interpenetrate helicoidal surfaces within an elongated enclosure.
• the interpenetrate helicoidal surfaces are on at least two screws extending along at least a portion of a longitudinal axis of the elongated enclosure.
• the process further comprising adjusting a rotational speed of the at least two screws to obtain the resinous mixture.
• the rotational speed of the at least two screws is between about 10 rpm and about 1000 rpm, preferably between 100 rpm and 200 rpm.
• said elongated enclosure comprises a plurality of sections corresponding to longitudinal segments of the at least two screws.
• the process further comprising controlling a temperature in at least one section of the plurality of sections.
• the temperature in each section of the plurality of sections is independently selected in the range of from about 20°C to about 170°C.
• the plurality of sections includes at least one mixing section and at least one conveying section. • the at least one mixing section is maintained at a first temperature and the least one conveying section is maintained at a second temperature, the first and second temperatures being different.
• the plurality of sections includes at least one reverse flow section.
• at least a first section of the plurality of sections comprises a first inlet for providing the isolated trichomes.
• at least a second section of the plurality of sections comprises a second inlet for providing one or more additional component(s).
• the one or more additional component(s) include one or more cannabinoid, one or more terpene, one or more flavonoid, one or more flavoring agent, water, one or more non-toxic coloring agent, or a mixture thereof.
• the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
• the one or more cannabinoid(s) includes a plurality of cannabinoids.
• the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
• the process further comprising cutting the hashish product according to a pre-established cutting operational parameter.
• the cutting pattern includes cutting the hashish product along a transverse axis to obtain pieces thereof of identical length and/or weight.
• the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%.
• the isolated cannabis trichomes are from a single cannabis strain. the isolated cannabis trichomes are from a plurality of cannabis strains. • the hashish product comprises a moisture content of from about 2 wt.% to about 8 wt.%, or of from about 2 wt.% to about 5 wt.%.
• the isolated trichomes are dry-sift kief.
[0014] In a broad aspect, the present disclosure relates to a hashish product comprising a substantially homogeneous cohesive mass of isolated cannabis trichomes made by the process described above.
[0015] In a broad aspect, the present disclosure relates to a hashish product comprising a substantially homogeneous cohesive mass of isolated cannabis trichomes having a % reflectance of at least 4%85.
[0016] In specific embodiments, the hashish product may include one or more of the following features:
• the hashish product has a lightness value L* £ 50 on CIELAB scale, or a lightness value L* from 0 to about 40, of from about 10 to about 30, of from about 15 to about 25.
• the hashish product has a % reflectance of at least 4.5%85, at least 5%85, or at least 5.5%85.
• comprising one or more additional component(s) selected from one or more cannabinoid, one or more terpene, one or more flavonoid, one or more flavoring agent, one or more non-toxic coloring agent, and any mixtures thereof.
• the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
• the one or more cannabinoid(s) includes a plurality of cannabinoids.
• the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
• the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%. the isolated cannabis trichomes are from a single cannabis strain.
• the isolated cannabis trichomes are from a plurality of cannabis strains.
• the hashish product comprises a moisture content of from about 2 wt.% to about 8 wt.%, or of from about 2 wt.% to about 5 wt.%.
• the isolated trichomes are dry-sift kief.
[0017] In a broad aspect, the present disclosure relates to process of making a hashish product, comprising providing isolated cannabis trichomes; mixing the isolated cannabis trichomes while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture; and retrieving at least a portion of the resinous mixture through an extrusion die to obtain the hashish product, wherein the hashish product has a moisture content of no more than about 8 wt.%.
[0018] In another broad aspect, the present disclosure relates to a process of making a hashish product, comprising providing isolated cannabis trichomes; mixing the isolated cannabis trichomes while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture; and retrieving at least a portion of the resinous mixture through an extrusion die to obtain the hashish product, wherein the hashish product is free of exogenous water.
[0019] In specific embodiments, the processes described above may include one or more of the following features:
• the moisture content of the hashish product is less than 8 wt.%.
• the moisture content of the hashish product is less than 5 wt.%.
• the moisture content of the hashish product is at least 2 wt.%.
• the hashish product has a lightness value L* £ 50 on CIELAB scale, preferably from 0 to about 40, or of from about 10 to about 30, or of from about 15 to about 25.
• the hashish product has a % reflectance of at least 4%85.
• the % reflectance of the hashish product is at least 4.5%85, at least 5%85, or at least
5.5%85. • the mixing includes applying compression and shear forces to the isolated trichomes via a plurality of interpenetrate helicoidal surfaces within an elongated enclosure.
• the interpenetrate helicoidal surfaces are on at least two screws extending along at least a portion of a longitudinal axis of the elongated enclosure.
• the process further comprises adjusting a rotational speed of the at least two screws to obtain the resinous mixture.
• the rotational speed of the at least two screws is between about 10 rpm and about 1000 rpm, preferably between 100 rpm and 200 rpm.
• the elongated enclosure comprises a plurality of sections corresponding to longitudinal segments of the at least two screws.
• the process further comprises controlling a temperature in at least one section of the plurality of sections.
• the temperature in each section of the plurality of sections is independently selected in the range of from about 20°C to about 170°C.
• the plurality of sections includes at least one mixing section and at least one conveying section.
• the at least one mixing section is maintained at a first temperature and the least one conveying section is maintained at a second temperature, the first and second temperatures being different.
• the plurality of sections includes at least one reverse flow section.
• at least a first section of the plurality of sections comprises a first inlet for providing the isolated trichomes.
• at least a second section of the plurality of sections comprises a second inlet for providing one or more additional component(s). • the one or more additional component(s) include one or more cannabinoid, one or more terpene, one or more flavonoid, one or more flavoring agent, one or more non-toxic coloring agent, or a mixture thereof.
• the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
• the one or more cannabinoid(s) includes a plurality of cannabinoids.
• wherein the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
• the process further comprises cutting the hashish product according to a pre-established cutting operational parameter.
• the cutting pattern includes cutting the hashish product along a transverse axis to obtain pieces thereof of identical length and/or weight.
• the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%.
• the isolated cannabis trichomes are from a single cannabis strain.
• the isolated cannabis trichomes are from a plurality of cannabis strains.
• the isolated trichomes are dry-sift kief.
• the hashish product is free of mold after a plurality of weeks.
[0020] In a broad aspect, the present disclosure relates to a hashish product comprising a substantially homogeneous cohesive mass of isolated cannabis trichomes made by one of the processes described above.
[0021] In a broad aspect, the present disclosure relates to a hashish product comprising an extruded, substantially homogeneous cohesive mass of isolated cannabis trichomes having a moisture content of no more than about 8 wt.%. [0022] In another broad aspect, the present disclosure relates to a hashish product comprising an extruded, substantially homogeneous cohesive mass of isolated cannabis trichomes that is free of exogenous water during extrusion.
[0023] In specific embodiments, the hashish products may include one or more of the following features:
• the moisture content of the hashish product is less than 8 wt.%.
• the moisture content of the hashish product is less than 5 wt.%.
• the moisture content of the hashish product is at least 2 wt.%.
• the hashish product has a lightness value L* £ 50 on CIELAB scale, preferably from 0 to about 40, or of from about 10 to about 30, or of from about 15 to about 25.
• the hashish product has a % reflectance of at least 4%85.
• the % reflectance of the hashish product is at least 4.5%85, at least 5%85, or at least 5.5%85.
• the hashish product comprises one or more additional component(s) selected from one or more cannabinoid, one or more terpene, one or more flavonoid, one or more flavoring agent, one or more non-toxic coloring agent, and any mixtures thereof.
• the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
• the one or more cannabinoid(s) includes a plurality of cannabinoids.
• the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
• the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%. the isolated cannabis trichomes are from a single cannabis strain. the isolated cannabis trichomes are from a plurality of cannabis strains.
• the isolated trichomes are dry-sift kief.
[0024] All features of exemplary embodiments which are described in this disclosure and are not mutually exclusive can be combined with one another. Elements of one embodiment can be utilized in the other embodiments without further mention. Other aspects and features of the present invention will become apparent to those ordinarily skilled in the art upon review of the following description of specific embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] The patent or application file contains at least one drawing executed in color. Copies of this patent or patent application publication with color drawing(s) will be provided by the Office upon request and payment of the necessary fee.
[0026] A detailed description of specific exemplary embodiments is provided herein below with reference to the accompanying drawings in which:
[0027] FIG. 1 illustrates a non-limiting flowchart example of a process for making a hashish product in accordance with an embodiment of the present disclosure;
[0028] FIG. 2 illustrates a non-limiting flowchart example of steps for obtaining isolated cannabis trichomes in accordance with an embodiment of the present disclosure;
[0029] FIG. 3 illustrates a non-limiting flowchart example of a process for working the resinous mixture from FIG 1 in accordance with an embodiment of the present disclosure;
[0030] FIG. 4 illustrates a non-limiting system implementing a process for making a hashish product in accordance with an embodiment of the present disclosure;
[0031] FIG. 5 illustrates a non-limiting schematic of a setting for performing a gloss and reflectance measurement;
[0032] FIG. 6A-6E are images of hashish product samples manufactured in accordance with Examples described herein; [0033] FIG. 7 A is a comparative image comparing hashish product samples manufactured with a single-screw extruder (I) and a double-screw extruder (II); and
[0034] FIG. 7B is a comparative image comparing hashish product samples manufactured with pressing (I), single-screw extruder (II), and double-screw extruder (III).
[0035] In the drawings, exemplary embodiments are illustrated by way of example. It is to be expressly understood that the description and drawings are only for the purpose of illustrating certain embodiments and are an aid for understanding. They are not intended to be a definition of the limits of the invention.
DETAILED DESCRIPTION
[0036] A detailed description of one or more embodiments is provided below along with accompanying figures that illustrate principles of the disclosure. The invention is described in connection with such embodiments, but the invention is not limited to any embodiment. The scope of the invention is limited only by the claims. Numerous specific details are set forth in the following description to provide a thorough understanding of the invention. These details are provided for the purpose of non-limiting examples and the invention may be practiced according to the claims without some or all these specific details. Technical material that is known in the technical fields related to the invention has not been described in detail so that the disclosure is not unnecessarily obscured.
[0037] The present inventors have developed a hashish product and industrial method of manufacturing same that addresses at least some of the above-identified problems.
[0038] For example, it has been observed that the hashish product according to the present disclosure has a visual appearance that substantially matches the consumer appealing hand made products without systematic use of exogenous ingredients (such as coloring agents, oils, etc.) and/or additional post-manufacturing processing performed by the manufacturer or user to artificially impart such visual appearance. For example, the industrial hash of the present disclosure can be characterized with dark color and shiny appearance, as would be expected from a hand-rubbed hashish, or bubble hashish, or hash made with high potency kief.
[0039] The present inventors have developed an industrial manufacturing process to produce such hash product that includes mixing isolated cannabis trichomes under specific conditions that are sufficient to obtain a resinous mixture which upon retrieval through an extrusion die affords a hashish product having the desired appearance. In other words, the process allows to have a shiny hash straight out of the die, without requiring further processing (e.g., rolling up as a ball, adding exogenous ingredients such as oils, etc.). Further, and in contrast to previous processes developed by the Applicant, it was surprisingly and unexpectedly discovered here that incorporating water into the kief was not necessary to produce hashish product having the desirable characteristics. This was surprising in view of specific pressing embodiments described in PCT Application Publication WO2021/119817, filed on December 16, 2020, and specific mixing embodiments described in PCT Application Publication WO2021/226725, filed on May 17, 2021 , which both incorporated water into kief to impart desirable characteristics to the resulting hash product.
[0040] Such difference also afforded a technical effect in that the resulting hash product can also be characterized as having a low moisture content, which can reduce or avoid likelihood of mold growth over time, thus affording advantageous extended shelf life to the hashish product compared to other industrial hashish with higher moisture content.
[0041] Such extended shelf life, observed with the hash of the present disclosure may also afford a technical effect in that this may avoid or minimize the need for irradiation (e.g., electron beams, x-rays or gamma rays). While irradiation is commonly used on food products to eliminate microorganism and thus extend shelf life, using irradiation on hashish products may be problematic for a number of reasons. For example, irradiation can be costly and time-consuming, especially multiple steps/doses of irradiation are implemented and/or if irradiation treatments are performed at an offsite location, which adds logistics to the overall costs.
[0042] These and other advantages may become apparent to the person of skill in view of the present disclosure.
Hashish Product
[0043] The hashish product of the present disclosure comprises a cohesive mass of isolated cannabis trichomes.
[0044] For example, the cohesive mass may be a substantially homogeneous cohesive mass of isolated trichomes. By “substantially homogeneous”, it is meant that the hashish product has a constant or uniform distribution of isolated trichomes throughout its cohesive mass. In other words, the manufacturing procedures described herein, process the isolated trichomes in such fashion to result in mixing thereof into a substantially constant, uniform cohesive mass.
[0045] As used herein, the term “cannabis trichomes” generally refers to crystal-shaped outgrowths or appendages (also called resin glands) on cannabis plants typically covering the leaves and buds. Trichomes produce hundreds of known cannabinoids, terpenes, and flavonoids that make cannabis strains potent, unique, and effective.
[0046] As used herein, the term “isolated cannabis trichomes” refers to trichomes that have been separated from cannabis plant material using any method known in the art. The details of various methods for separating trichomes from the cannabis plant are well-known in the art. For example, and without wishing to be limiting in any manner, the isolated cannabis trichomes may be obtained by manual processes like dry sifting or by water extraction methods. Solvent-less extraction methods can include mechanical separation of trichomes from the plant, such as sieving through a screen by hand or in motorized tumblers (see for example WO 2019/161509), or by submerging the cannabis plants in icy water (see for example US2020/0261824, which is herein incorporated by reference) and agitating to separate the trichomes from the plant and drying the trichomes. Because of inherent limitations to existing separation methods, some plant matter or other foreign matter can be present in isolated cannabis trichomes.
[0047] Isolated cannabis trichomes obtained by mechanical separation of trichomes from the cannabis plant biomass is typically referred to as “kief’ (also “keef” or “kif”) and has a powdery appearance. Typically, some residual plant material remains in the finished kief and thus in the resulting hashish product. In some embodiments, the isolated trichomes are dry-sift kief.
[0048] The isolated cannabis trichomes forming the hashish product of the present disclosure may originate from one or more than one strain of cannabis plant. It is known amongst consumers of hashish and other cannabis products that using isolated cannabis trichomes produced from more than one strain of cannabis plant allows a user to tune the psychoactive and/or entourage effect obtained by consuming the product. The mixing of cannabis plant strains may also allow to adjust the final concentration of a component of the product, for example but not limited to the cannabinoid content. Additionally, use of more than one strain allows for improved product and waste management - important in commercial production.
[0049] As used herein, the term “cannabis” generally refers to a genus of flowering plants that includes several species. The number of species is currently being disputed. There are three different species that have been recognized, namely Cannabis sativa, Cannabis indica and Cannabis ruderalis. Hemp, or industrial hemp, is a strain of the Cannabis sativa plant species that is grown specifically for the industrial uses of its derived products. In terms of cannabinoids content, hemp has lower concentrations of tetrahydrocannabinol (THC) and higher concentrations of cannabidiol (CBD), which decreases or eliminates the THC-associated psychoactive effects.
[0050] In some embodiments, the hashish product of the present disclosure is characterized as having a desirable dark color, such as having a lightness value L* £ 50 on CIELAB scale.
[0051] The person of skill will readily understand that assessing and/or measuring the color can be performed quantitatively using a colorimeter, a spectrophotometer, or qualitatively with the human eye. For example, for quantitative assessment / measurement, the color can be measured by reflectance spectrophotometer ASTM standard test methodology. Tristimulus L*, a*, b* values are measured from the viewing surface of the hashish product. These L*, a*, b* values are reported in terms of the CIE 1976 color coordinate standard (CIELAB scale). L* is lightness which is the relative brightness of a surface with a range from 0-100, wherein L*=0 translates as darkest black and L*=100 translates as lightest white.
[0052] In some embodiments, the hashish product of the present disclosure has a lightness value L* £ 50 based on the CIELAB scale - e.g., the reader will readily recognize that such lightness value range leaves flexibility to the producer, as the product can be made darker through other means if desirable to favor consumer appeal.
[0053] For example, the hashish product may have a lightness value L* from 0 to about 50 or any value therebetween, or in a range of values defined by any values therebetween. For example, the hashish product may have a lightness value L* up to about 50, up to about 45, up to about 40, up to about 35, up to about 30, up to about 25, up to about 20, up to about 15, up to about 10, up to about 5 or any value therebetween. For example, the hashish product may have a lightness value L* of from about 5 to about 45, of from about 10 to about 40, from about 15 to about 35, from about 20 to about 30. For example, the hashish product may have a lightness value L* of about 5, of about 10, of about 15, of about 20, of about 25, of about 30, of about 35, of about 40, of about 45, or about 50.
[0054] In some embodiments, the hashish product of the present disclosure is characterized as having a desirable shininess, such as having a % reflectance of at least about 5%85. [0055] The person of skill will readily understand that reflectance is the proportional amount of reflected light measured from a sample surface, relative to the amount of reflected light measured from a reference plate and can thus serve to characterize the shininess of a hashish product.
[0056] %Reflectance can be determined in several ways all of which are known to the person skilled in the art. For example, %Reflectance could be determined by a glossmeter which initially determines shininess in terms of gloss by directing a constant intensity light beam, at a fixed angle Y, on to the test surface and monitoring the amount of reflected light from the same angle. The determined gloss value (also known as Gloss Unit or GU) is in turn translated to %reflectance. Whilst the Gloss Unit (GU) scale is linear, each angle of incidence has a different gloss measurement range; 0 - 2000 GU (for 20°), 0 - 1000 GU (for 60°) and 0 - 160 GU (for 85°). %Reflectance compares the amount of light energy transmitted and received by a glossmeter and expresses the value as a percentage of the angle of incident's full measurement range and the value is displayed as a percentage relative to the selected angle of incidence. For example, as the measurement range for a 20° glossmeter is 0-2000 GU; a value of 1000 GU at 20° would be expressed in terms of %reflectance as 50%20, and a value of 500 GU would be expressed as 25%20. However, A value of 500 GU at 60°, but would be expressed as 50%60 as the measurement range for the 60° is 0 - 1000 GU.
[0057] In one practical example gloss can be determined with the Elcometer™ 480 Model T glossmeter with integrated ElcoMaster™ software (Elcometer, USA). In order to determine the most appropriate measurement angle start with a gloss meter set at 60 degrees angle of incidence. If the result is between 10-70GU, the coating is termed ‘semi-gloss’ and should be measured using the 60 degrees angle. If the result is less than 10GU, the product is ‘low gloss’ and should be measured using the 85 degrees angle and if it is greater than 70GU, the product is known as ‘high gloss’ and should be measured using the 20 degrees angle.
[0058] In some embodiments, the hashish product according to the present disclosure has a gloss value of at least 6 GU, at least 7 GU, at least 8 GU, or even greater (e.g., at least 9 GU, at least 10 GU, or more).
[0059] For instance, in some embodiments, the hashish product according to the present disclosure has a %reflectance of at least 4%85, at least 4.5%85, at least 5%85, at least 5.5%85, or even greater (e.g., at least 6%85, at least 7%85, or more). [0060] Without being bound by any theory, it is believed that hashish shininess may depend on several factors, for example, the potency of the base materials, i.e. , for example water and ice isolation of kief has been reported to isolate kief of higher potency and higher purity, thus higher amounts of resin content capable of being oozed out which can favor obtaining shinier hash; the processing parameters to obtain the hash can affect the level of how much resin can be extracted from the trichomes, for example hand rubbing the hash may impart more mechanical / thermal energy to the kief thus extracting more resin therefrom compared to simply pressing the kief in an industrial press; post processing steps performed by the manufacturer and/or users, such as rolling the hashish product into a ball which has been reported to enhance the shiny aspect of hashish product that have sufficient resin content to expose at the outer surface of the hashish product; and the like. A common trait being that higher potency / higher resin content correlates with better cohesion and smoothness as well as desired color and/or shininess. It was thus surprising to the inventors to be able to obtain hash with such desirable shininess without recourse to such procedures known to favor shininess. For example, the present inventors were able to obtain hand-rubbed hash shininess levels using dry-sift kief with an extruder device, where dry- sift kief is known to produce less shiny hash.
[0061] While the manufacturing process described herein does not require incorporating water into kief, thus resulting in a hashish product having low moisture content - the resulting hash product can include a residual moisture content, which can originate for example from endogenous water present in the kief or other liquids, such as terpenes. In some embodiments, the hashish product of the present disclosure can comprise a moisture content of no more than about 8 wt.% (e.g., less than 8 wt.%), such as from about 2 wt.% to about 8 wt.% or any value therebetween, or in a range of values defined by any values therebetween. For example, the hashish product may have a moisture content of up to about 8 wt.%, of up to about 7 wt.%, of up to about 6 wt.%, of up to about 5 wt.%, of up to about 4 wt.%, of up to about 3 wt.%, or of up to about 2.5 wt.% or any value therebetween. For example, the hashish product may have a moisture content of from about 2.5 wt.% to about 4.5 wt.%, from about 2.8 wt.% to about 4.2 wt.%, from about 3.0 wt.% to about 4.0 wt.%, from about 3.2 wt.% to about 3.8 wt.%, or from about 3.4 wt.% to about 3.6 wt.%.
[0062] In specific implementations, the present inventors measured an about 2.5 wt.% drop in moisture from processing the kief through the mixing process described herein to obtain a hash product having the desired characteristics (e.g., dark black, shiny, and malleable). For example, in a specific embodiment, the present inventors obtained a hash product having moisture content of 3-5 wt.% using a dry-sift kief having an initial moisture content of 7.4 wt.%.
[0063] In some embodiments, water can be added into the process depending on specific applications. For example, water could be added to help more efficiently conduct thermal energy to the product and/or help form cohesive forces leading to a more malleable and soft texture. For example, water could be added in the form of liquid water, steam, or ice. For example, the water being added can be water purified using any known process, such as capacitive deionization, reverse osmosis, carbon filtering, microfiltration, ultrafiltration, ultraviolet oxidation, electrodeionization, distillation, and the like.
[0064] The moisture content of the hashish product can be determined by several methods known to the person skilled in the art including but not limited to Thermogravimetry Analysis (TGA) and equipment such as Mettler Toledo™ Hal. Moisture Analyzer HC103 (Fisher Scientific, USA) or MA160 Thermogravimetric Moisture Balance-type Analyzer (Sartorius Canada Inc).
Cannabinoid content
[0065] The hashish product of the present disclosure comprises one or more cannabinoid(s). The one or more cannabinoid(s) may be present endogenously in the isolated trichomes used to make the hash product or may be added in the form of an additional component (as described later in this text).
[0066] As used herein, the term “cannabinoid” generally refers to any chemical compound that acts upon a cannabinoid receptor such as CBi and CB2. Examples of cannabinoids include, but are not limited to, cannabichromanon (CBCN), cannabichromene (CBC), cannabichromevarin (CBCV), cannabicitran (CBT), cannabicyclol (CBL), cannabicyclovarin (CBLV), cannabidiol (CBD, defined below), cannabidiolic acid (CBDA), cannabidiol monomethylether (CBDM), cannabidiol- C4 (CBD-C4), cannabidiorcol (CBD-C1), cannabidiphorol (CBDP), cannabidivarin (CBDV), cannabielsoin (CBE), cannabifuran (CBF), cannabigerol (CBG), cannabigerol monomethylether (CBGM), cannabigerolic acid (CBGA), cannabigerovarin (CBGV), cannabinodiol (CBND), cannabinodivarin (CBVD), cannabinol (CBN), cannabinol methylether (CBNM), cannabinol propyl variant (CBNV), cannabinol-C2 (CBN-C2), cannabinol-C4 (CBN-C4), cannabiorcol (CBN-C1), cannabiripsol (CBR), cannabitriol (CBO), cannabitriolvarin (CBTV), cannabivarin (CBV), dehydrocannabifuran (DCBF), A7-cis-iso tetrahydrocannabivarin, tetrahydrocannabinol (THC, defined below), A9-tetrahydrocannabionolic acid B (THCA-B), A9-tetrahydrocannabinolic acid A (THCA-A), A9-tetrahydrocannabiorcol (THC-C1), tetrahydrocannabivarinic acid (THCVA), tetrahydrocannabivarin (THCV), ethoxy-cannabitriolvarin (CBTVE), trihydroxy-A9- tetrahydrocannabinol (triOH-THC), 10-ethoxy-9hydroxy-A6a-tetrahydrocannabinol, 8,9- dihydroxy-A6a-tetrahydrocannabinol, 10-oxo-A6a-tetrahydrocannabionol (OTHC), 3, 4,5,6- tetrahydro-7-hydroxy-a-a-2-trimethyl-9-n-propyl-2, 6-methano-2H-1-benzoxocin-5-methanol (OH-iso-HHCV), A6a,10a-tetrahydrocannabinol (A6a,10a-THC), Dd-tetrahydrocannabivarin (D8- THCV), A9-tetrahydrocannabiphorol (D9-THOR), A9-tetrahydrocannabutol (D9-THOB), derivatives of any thereof, and combinations thereof. Further examples of suitable cannabinoids are discussed in at least WO2017/190249 and U.S. Patent Application Pub. No. US2014/0271940, which are each incorporated by reference herein in their entirety.
[0067] Cannabidiol (CBD) means one or more of the following compounds: A2-cannabidiol, D5- cannabidiol (2-(6-isopropenyl-3-methyl-5-cyclohexen-l-yl)-5-pentyl-l,3-benzenediol); D4- cannabidiol (2-(6-isopropenyl-3-methyl-4-cyclohexen-l-yl)-5-pentyl-l,3-benzenediol); D3- cannabidiol (2-(6-isopropenyl-3-methyl-3-cyclohexen-l-yl)-5-pentyl-l,3-benzenediol); D3,7- cannabidiol (2-(6-isopropenyl-3-methylenecyclohex-l-yl)-5-pentyl-l,3-benzenediol); D2- cannabidiol (2-(6-isopropenyl-3-methyl-2-cyclohexen-l-yl)-5-pentyl-l,3-benzenediol); D1- cannabidiol (2-(6-isopropenyl-3-methyl-l-cyclohexen-l-yl)-5-pentyl-l,3-benzenediol); and D6- cannabidiol (2-(6-isopropenyl-3-methyl-6-cyclohexen-l-yl)-5-pentyl-l,3-benzenediol). In a preferred embodiment, and unless otherwise stated, CBD means A2-cannabidiol.
[0068] Tetrahydrocannabinol (THC) means one or more of the following compounds: D8- tetrahydrocannabinol (Dd-THC), Dd-tetrahydrocannabivarin (Dd-THCV), A9-cis- tetrahydrocannabinol (cis-THC), A9-tetrahydrocannabinol (D9-THO), D10-tetrahydrocannabinol (DIO-THC), A9-tetrahydrocannabinol-C4 (THC-C4), A9-tetrahydrocannabinolic acid-C4 (THCA- C4), synhexyl (n-hexyl-A3THC). In a preferred embodiment, and unless otherwise stated, THC means one or more of the following compounds: A9-tetrahydrocannabinol and D8- tetrahydrocannabinol.
[0069] In one embodiment, the hashish product of the present disclosure contains the one or more cannabinoid(s) in an amount sufficient for the user to experience a desired effect when consuming the product. For example, the hashish product may comprise from about 5 wt.% to about 90 wt.% cannabinoid or any value therebetween, or in a range of values defined by any values therebetween. For example, the hashish product may comprise up to about 90 wt.%, up to about 80 wt.%, up to about 70 wt.%, up to about 60 wt.%, or up to about 50 wt.%, or up to about 40 wt.%, or up to about 30 wt.% or any value therebetween, or in a range of values defined by the aforementioned values. For example, the hashish product may comprise from about 10 wt.% to about 60 wt.%, more preferably from about 20 wt.% to about 50 wt.%. In another embodiment, the hashish product may include up to 1000 mg/g THC, depending on specific implementations of the present disclosure.
[0070] In some embodiments, alternatively or additionally, the hashish product of the present disclosure may include one or more cannabinoid, such as THC, CBD, CBG, CBN, or any combinations thereof. For example, the THC can be delta-9-THC and/or delta-8-THC. The cannabinoids can be in similar or different amounts, depending on specific implementations of the present disclosure.
[0071] A cannabinoid may be in an acid form or a non-acid form, the latter also being referred to as the decarboxylated form since the non-acid form can be generated by decarboxylating the acid form.
[0072] The content in the acid form and the decarboxylated form of a specific cannabinoid can be determined using suitable methods known to the person skilled in the art, such as but not limited to Gas Chromatography/ Mass Spectrometry (GC/MS), High Performance Liquid Chromatography (HPLC), Gas Chromatography/ Flame Ionization Detection (GC/FID), Fourier transform infrared (FT-IR) spectroscopy, and the like. Various suitable methods are described, for example, in Formato et al. (-)-Cannabidiolic Acid, a Still Overlooked Bioactive Compound: An Introductory Review and Preliminary Research. Molecules. 2020 Jun 5;25(11):2638.
Additional components
[0073] The hashish product according to the present disclosure may also comprise one or more additional components.
[0074] In some embodiments, the one or more additional components may be added to alter the characteristics of the hashish product, such as cannabinoid content, potency, entourage effect, odor, color, shine, consistency, texture, malleability, and the like.
[0075] In some embodiments, the one or more additional components may be substantially homogeneously distributed on at least a portion of a surface of the hashish product, for example as a coating, and/or the one or more additional components may be substantially homogeneously distributed throughout the cohesive mass forming the hash product. For example, the portion of the surface of the hashish product may include at least 20%, at least 30%, at least 40%, at least 50%, at least 60%, at least 70%, at least 80%, at least 90%, or 100% of the surface of the hashish product.
[0076] The one or more additional component may be any suitable food grade and/or non-toxic composition or component known in the art. As will be recognized by those of skill in the art, the toxicity of each type of additional component may be dependent on the method of consumption of the hashish product. For example, in applications where smoke / vapor produced by the hashish product is to be inhaled, suitable additional components may include, but are not limited to one or more cannabinoid, one or more terpene (also referred to herein as a “terpene blend”), water, one or more flavonoid, or any combination thereof.
[0077] The one or more additional component may be a cannabinoid. The cannabinoid may be extracted from any suitable source material including, but not limited to, cannabis or hemp plant material (e.g., flowers, seeds, and trichomes) or may be manufactured artificially (for example cannabinoids produced in yeast, as described in WO WO2018/148848). Cannabinoids can be extracted from a cannabis or hemp plant material according to any procedure known in the art. For example, and without wishing to be limiting, a “crude extract” containing a cannabinoid may be obtained by extraction from plant materials using for example aliphatic hydrocarbons (such as propane, butane), alcohols (such as ethanol), petroleum ether, naphtha, olive oil, carbon dioxide (including supercritical and subcritical CO2), chloroform, or any combinations thereof. Optionally, the crude extract may then be “winterized”, that is, extracted with an organic solvent (such as ethanol) to remove lipids and waxes (to produce a “winterized extract”), as described for example in US 7,700,368, US 2004/0049059, and US 2008/0167483, which are each herein incorporated by reference in their entirety. Optionally, the method for obtaining the cannabinoid may further include purification steps such as a distillation step to further purify, isolate or crystallize one or more cannabinoids, which is referred to in the art and herein as a “distillate”; US20160346339, which is incorporated herein by reference, describes a process for extracting cannabinoids from cannabis plant material using solvent extraction followed by filtration, and evaporation of the solvent in a distiller to obtain a distillate. The distillate may be cut with one or more terpenes. The crude extract, the winterized extract or the distillate may be further purified, for example using chromatographic and other separation methods known in the art, to obtain an “isolate”. Cannabinoid extracts may also be obtained using solvent-less extraction methods; for example, cannabis plant material may be subjected to heat and pressure to extract a resinous sap (“rosin”) containing cannabinoids; methods for obtaining rosin are well-known in the art. [0078] The one or more additional component may thus include one or more cannabinoid in the form of a crude cannabis extract, a cannabis distillate, a cannabis isolate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
[0079] The one or more additional component may be a terpene. As used herein, the term “terpene” generally refers to a class of chemical components comprised of the fundamental building block of isoprene, which can be linked to form linear structures or rings. Terpenes may include hemiterpenes (single isoprenoid unit), monoterpenes (two units), sesquiterpenes (three units), diterpenes (four units), sesterterpenes (five units), triterpenes (six units), and so on. At least some terpenes are expected to interact with, and potentiate the activity of, cannabinoids. Any suitable terpene may be used in the hashish product of the present invention. For example, terpenes originating from cannabis plant may be used, including but not limited to aromadendrene, bergamottin, bergamotol, bisabolene, borneol, 4-3-carene, caryophyllene, cineole/eucalyptol, p-cymene, dihydroj asmone, elemene, farnesene, fenchol, geranylacetate, guaiol, humulene, isopulegol, limonene, linalool, menthone, menthol, menthofuran, myrcene, nerylacetate, neomenthylacetate, ocimene, perillylalcohol, phellandrene, pinene, pulegone, sabinene, terpinene, terpineol, 4-terpineol, terpinolene, and derivatives thereof. Additional examples of terpenes include nerolidol, phytol, geraniol, alpha-bisabolol, thymol, genipin, astragaloside, asiaticoside, camphene, beta-amyrin, thujone, citronellol, 1,8-cineole, cycloartenol, hashishene, and derivatives thereof. Further examples of terpenes are discussed in US Patent Application Pub. No. US2016/0250270, which is herein incorporated by reference in its entirety for all purposes. The hashish product of the present disclosure may contain one or more terpene(s). The one or more terpene(s) may originate from the hashish, from an additional component, or both. In some embodiments, the hashish product of the present disclosure may include the one or more terpene(s) in an amount (the “terpene content”) sufficient for the user to experience a desired entourage effect when consuming the product. For example, the hashish product may comprise from about 0.5 wt.% to about 15 wt.% terpene, for example up to about 15 wt.%, or up to about 10 wt.%, or up to about 5 wt.%, or up to about 4 wt.%, or up to about 3 wt.%, or up to about 2 wt.%, or up to about 1 wt.%. For example, the one or more terpene(s) may include hashishene. Without wishing to be bound by theory, hashishene is believed to be a terpene produced by rearrangement of myrcene that may be found in hashish after mechanical processing, and that may be responsible for the typical desirable “hashish flavour”. [0080] The one or more additional component may be a flavonoid. The term “flavonoid” as used herein refers to a group of phytonutrients comprising a polyphenolic structure. Flavonoids are found in diverse types of plants and are responsible for a wide range of functions, including imparting pigment to petals, leaves, and fruit. Any suitable flavonoid may be used in the hashish product of the present invention. For example, flavonoids originating from a cannabis plant may be used, including but not limited to: apigenin, cannflavin A, cannflavin B, cannflavin C, chrysoeril, cosmosiin, flavocannabiside, homoorientin, kaempferol, luteolin, myricetin, orientin, quercetin, vitexin, and isovitexin.
[0081] The reader will readily understand that in some implementations, the one or more additional component may include a combination of any one of the one or more additional component described herein.
Consumer use of hashish products
[0082] As is known in the art, hashish is typically used for recreational or medicinal uses. For example, hashish products can be used to achieve a desired effect in a user, such as a psychoactive effect, a physiological effect, or a treatment of a condition. By “psychoactive effect”, it is meant a substantial effect on mood, perception, consciousness, cognition, or behavior of a subject resulting from changes in the normal functioning of the nervous system. By “physiological effect”, it is meant an effect associated with a feeling of physical and/or emotional satisfaction. By “treatment of a condition”, it is meant the treatment or alleviation of a disease or condition by absorption of cannabinoid(s) at sufficient amounts to mediate the therapeutic effects.
[0083] The terms “treating”, “treatment” and the like are used herein to mean obtaining a desired pharmacologic and/or physiologic effect. The effect may be prophylactic, in terms of completely or partially preventing a disease, condition, or symptoms thereof, and/or may be therapeutic in terms of a partial or complete cure for a disease or condition and/or adverse effect, such as a symptom, attributable to the disease or disorder. “Treatment” as used herein covers any treatment of a disease or condition of a mammal, such as a dog, cat or human, preferably a human.
[0084] In certain embodiments, the disease or condition is selected from the group consisting of pain, anxiety, an inflammatory disorder, a neurological disorder, a psychiatric disorder, a malignancy, an immune disorder, a metabolic disorder, a nutritional deficiency, an infectious disease, a gastrointestinal disorder, and a cardiovascular disorder. Preferably the disease or condition is pain. In other embodiments, the disease or condition is associated with the feeling of physical and/or emotional satisfaction.
[0085] In the context of recreational use, the “effective amount” administered and rate and time- course of administration, will depend on the desired effect associated with a feeling of physical and/or emotional satisfaction in the subject.
[0086] In the context of health and wellness use, the “effective amount” administered, and rate and time-course of administration will depend on the nature and severity of the disease or condition being treated and typically also takes into consideration the condition of the individual subject, the method of administration and the like.
Manufacturing process
[0087] The hashish product may be produced by mixing the components thoroughly to provide a resinous mixture having desired characteristics.
[0088] For example, the mixing may be performed by mechanically mixing. By the term “mechanically mixing” or “mechanical mixing”, it is meant mixing using any suitable mechanical means. The mechanical means may be, for example, a plurality of interpenetrate helicoidal surfaces within an elongated enclosure or barrel, a non-limiting example of which is an extruder apparatus.
[0089] An extruder apparatus is a machine used to perform an extrusion process. Manufacturing by extrusion occurs when a material (usually pellets, dry powder, rubber, plastic, metal bar stock or food) is heated and pushed through a die assembly. A die is a mold that shapes the heated material as it is forced through a small opening from the inside of the extruder to the outside. Using a system of barrels or cylinders containing interpenetrate helicoidal surfaces, e.g., screw pumps or extruder screws, the extruder can mix the ingredients, and optionally adding heating, while propelling the extrudate through the die, for example to impart a desired shape to the hashish product. Extruders use in the industry are often of single-screw or twin-screw type.
[0090] Twin-screw extruders are known in the art - screws of such extruders may be parallel or non-parallel, converging or non-converging, with or without differential speed, counter or non counter rotating as described for example in US 6,609,819, WO 2020/220390, WO 2020/220495 and US 2010/0143523, where each of which is herein incorporated by reference in its entirety. It will be readily appreciated that extruders have flexible configuration (in terms of mixing zones, temperature zones, input zones, etc.) and that any suitable configuration of an extruder apparatus capable of producing a hashish product may be used within the context of the present disclosure.
[0091] A twin-screw extruder can be configured to have one or more mixing zones, one or more conveying zones, or one or more compression zones. Each of the zones may have input ports used for introduction of material. The mixing zones apply shear forces to the input materials, blending until they are homogenized. The extruder die assembly may perform a variety of functions: it may form or shape the extrudate, it may divide the extrudate into multiple extrudates, it may inject one or more component into the extrudate, and it may compress and reduce the cross-sectional area of the extrudate. It will be readily appreciated that extruders have flexible configuration (in terms of mixing zones, conveying zones, compression zones, etc.) and that any suitable configuration of an extruder apparatus (with any axial temperature profile or with any number of input ports) capable of producing a hashish product may be used within the context of the present disclosure.
[0092] As discussed later in this text, double screw extruders tested herein were more efficient than single screw extruders or industrial presses to impart the desired characteristics to the hashish in absence of water addition to the kief. Without being bound by any theory, it is believed that water addition when pressing or mixing may be required to provide a means to enhance heat transfer, which is necessary for trichome resin to ooze out, thus affording better product cohesion and smoothness, and for facilitating cannabinoid decarboxylation. In the present case, it was surprisingly discovered that the manufacturing process described herein manages to increase heat transfer efficiency without addition of water. For example, the present manufacturing process can achieve high heat and shear sufficient to obtain the desired hashish characteristics. In some embodiments, such high heat and shear can be created from mechanical mixing elements such as mixing pins and/or reverse flow elements. The reverse flow elements can increase the retention time of material on the mixing elements that it precedes. The mixing pins and reverse flow elements collectively can result in a tightly packed area that contributes to an increase in heat transfer efficiency. Such configurations can thus afford darker and shinier hashish product compared to hashish product manufactured with industrial press or single screw extruder.
[0093] FIG. 1 is a non-limiting flowchart of a process 100 for making a hashish product in accordance with an embodiment of the present disclosure. The process 100 comprises a first step 110 of providing isolated cannabis trichomes. [0094] In one non-limiting example, the isolated cannabis trichomes may include trichomes isolated from a single cannabis strain. In another non-limiting example, the isolated cannabis trichomes may include trichomes isolated from a plurality of distinct cannabis strains, which may have different respective cannabinoid(s) and/or terpene(s) content. The choice of one over the other may be driven by practical considerations, such as but not limited to inventory management considerations, the desired cannabinoid content of the hashish product, the desired user experience, and the like. It is known amongst consumers of hashish and other cannabis products that using isolated cannabis trichomes produced from more than one strain of cannabis plant may allow a user to tune the psychoactive, medical and/or entourage effect obtained by consuming the product. The mixing of cannabis plant strains may also allow adjustments to the final concentration of a component of the product, for example but not limited to the cannabinoid content. Additionally, use of more than one strain allows for improved product and waste management - important in commercial production.
[0095] The isolated cannabis trichomes may be obtained in several ways.
[0096] The producer implementing the process 100 may obtain the isolated cannabis trichomes from another producer. The step 110 may thus include a sub-step of obtaining the isolated cannabis trichomes from another producer (not shown in figures).
[0097] Alternatively, the producer implementing the process 100 may obtain the isolated cannabis trichomes via the following variants of step 110.
[0098] FIG. 2 is a variant 110’ which includes starting from cannabis plant material to isolate the cannabis trichomes therefrom. In this variant, a first step 210 includes providing cannabis plant material comprising cannabis trichomes. The cannabis plant material may comprise cannabis flowers / buds, cannabis trim, cannabis leaves, or any combination thereof. The producer implementing the first variant step 110’ may also produce the cannabis plant material or may obtain the cannabis plant material from another producer. In a second step 220, cannabis trichomes are isolated therefrom, thus resulting in the isolated cannabis trichomes. As discussed previously, various processes for isolating cannabis trichomes from cannabis plant material are known and as such, will not be further described here.
[0099] In some embodiments, the variant step 110’ may be performed at a first location while the remaining steps of process 100 may be performed at a second location, where the first and second locations may be within the same licensed producer site or within different licensed producer sites. In some embodiments, all steps of process 100 may be performed at the same location.
Mixing isolated cannabis trichomes and retrieving through a die
[0100] Returning to Fig. 1 , the process 100 further comprises a step 130 of mixing the isolated cannabis trichomes. In one practical implementation, the mixing includes applying compression and shear forces to the isolated cannabis trichomes via a plurality of interpenetrate helicoidal surfaces within an elongated enclosure. Preferably, the elongated enclosure is an extruder device having at least two screws. The isolated cannabis trichomes are mixed while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture.
[0101] For example, the resinous mixture is a substantially homogeneous mixture.
[0102] The conditions to form the resinous mixture at the mixing step 130 comprise shear, pressure, and temperature, which may be varied to alter the characteristics of the hashish product. Such characteristics may include, but without being limited to homogeneity, lightness, %reflectance, stiffness (i.e. , characteristic that defines the level of malleability of the hashish product), hardness or resistance to localized deformation (i.e., characteristic that determines how easy it is to cut or separate the hashish product), toughness (i.e., characteristic that determines the likelihood that the hashish product deforms rather than fractures under an applied force), color, tactual characteristics, and the like.
[0103] For example, the pressure being applied at the mixing step 130 may be at a value of about 1 bar or more. For example, a pressure of from about 1 bar to about 70 bar, including any ranges therein or any value therein. For example, a pressure of from about 1 bar to about 65 bar, from about 3 bar to about 60 bar, from about 4 bar to about 55 bar, from about 6 bar to about 50 bar, from about 8 bar to about 45 bar, from about 10 bar to about 40 bar, from about 12 bar to about 35 bar, from about 12 bar to about 32 bar, from about 14 bar to about 30 bar, from about 16 bar to about 28 bar, from about 18 bar to about 26 bar, or from about 20 bar to about 24 bar including any ranges therein or any value therein. For example, a pressure of about 1 bar, about 3 bar, about 4 bar, about 5 bar, about 8 bar, about 10 bar, about 12 bar, about 14 bar, about 16 bar, about 18 bar, about 22 bar, about 22 bar, about 24 bar, about 26 bar, about 28 bar, about 30 bar, about 32 bar, about 35 bar, about 40 bar, about 45 bar, about 50 bar, about 55 bar, about 60 bar, or around 65 bar. The person of skill will readily understand that a given pressure value may be selected depending on the die that is used to form the hashish product, as described elsewhere in this text.
[0104] For example, the temperature being applied at the mixing step 130 may be at a value of about 170°C or less. For example, a temperature of from about 20°C to about 170°C, including any ranges therein or any value therein. For example, a temperature of about 20°C, about 25°C, about 30°C, about 35°C, about 40°C, about 45°C, about 50°C, about 55°C, about 60°C, about 65°C, about 70°C, about 80°C, about 90°C, about 100°C, about 110°C, about 120°C, about 130°C, about 140°C, about 150°C, about 160°C, or about 170°C. It will be readily apparent to the person skilled in the art that different temperatures corresponding to the abovementioned temperature values or ranges may be used in different zones during the process as described elsewhere in this text.
[0105] The mixing shear and compressive forces can be controlled by modulating the rotational speed of the screws within the extruder. In such embodiments, the extruder screws rotation per minute (rpm) can be selected to perform the mixing step 130 at a value of for example about 10 rpm or more. For example, extruder screws rpm can be selected in a range of from about 10 rpm to about 1000 rpm, including any ranges therein or any value therein. For example, from about 15 to about 500 rpm, or from about 25 to about 450 rpm, or from about 30 to about 400 rpm, or from about 45 to about 450 rpm including any value within any of these ranges and preferably between 100 rpm and 200 rpm.
[0106] In embodiments where the heating and mixing are performed in a twin-screw extruder, the residence time within the extruder barrel can be directly related to the length of the barrel and the rotational speed of the twin screws. To increase mixing time of the components within the barrel, the components can travel through at least one zone of the barrel in a distal direction, and then be redirected to at least one zone of the barrel in a proximal direction (i.e., towards the inlet rather than towards the die).
[0107] Optional step 120 includes incorporating one or more additional component at one or more steps during the process 100. For example, one or more additional component can be added to the isolated trichomes prior to, simultaneously with, or following step 110, or prior to, simultaneously with, or following the mixing step 130. Multiple additional components may be added in a single step or may be added separately in one or more consecutive steps or at different times or points along the process 100. The one or more additional components can be one or more cannabinoids, one or more terpenes, one or more flavonoids, one or more flavoring agents, one or more non-toxic coloring agents, or any combination thereof. When the one or more component comprises a cannabinoid, the cannabinoid may be provided in the form of a cannabis extract (including a crude extract, or a winterized extract), a distillate, an isolate, cannabis rosin, cannabis resin, cannabis wax, or cannabis shatter.
[0108] In some embodiments, the one or more additional component may be incorporated during the process (through one or more input ports located at each of the zones within the extruder length, as described elsewhere in this text) to produce the hashish product.
[0109] For example, the one or more additional component may be substantially homogeneously distributed throughout the hashish product.
[0110] Once the resinous mixture is obtained at step 130, at least a portion of the resinous mixture is retrieved at step 140 to obtain an individual unit of hashish product having a cohesive mass of the isolated trichomes.
[0111] For example, the hashish product may have a substantially homogeneous cohesive mass of the isolated trichomes.
[0112] FIG. 3 includes additional steps that can follow step 140 of the process 100 in FIG. 1. For example, the at least portion of the resinous mixture can be passed through a die at step 150, which may be configured to impart a pre-determined shape thereto. Optionally, and prior to passing through the die, the at least portion of the resinous mixture may be cooled at step 145. The solid or semi-solid hashish product from step 150, may optionally further undergo post processing steps. For example, the solid or semi-solid hashish product from step 150 may be cut to a pre-determined cutting pattern, a pre-determined weight, or a pre-determined length to obtain smaller units of hashish product for a pre-determined packaging size (not shown in the figures).
Practical implementation
[0113] There are several options to implement the herein described process 100.
[0114] FIG. 4 illustrates a system 400 for implementing the process 100 to make a coherent and cohesive mass 480 in accordance with an embodiment. The system 400 includes an extruder apparatus 410 that uses mechanical mixing means to amalgamate the isolated cannabis trichomes 420 into the coherent and cohesive mass 480. [0115] In this embodiment, the system 400 comprises a feed hopper 425 through which the isolated cannabis trichomes 420 are fed. Optionally, one or more additional component(s) 440 are fed through the feed hopper 425 and/or through one or more input port 445 located along the length of the apparatus 410 at locations corresponding to one or more predetermined portions or zones 450A-G of the extruder apparatus 410. As discussed previously, non-limiting examples of such one or more additional component(s) 440 include, for example, terpenes, flavonoids, cannabinoids in the form of crude extracts, distillates, isolates, winterized cannabis extracts, rosin, shatter, or resins, or any combinations thereof.
[0116] The extruder apparatus 410 is powered by a motor (not shown) that drives at least two extruder screws 430 to apply pressure and mechanical shear on the isolated cannabis trichomes 420 and optionally the one or more additional component(s) 440 entering the extruder 410 (for the sake of brevity only one screw of the twin-screw is illustrated in Fig. 4). For example, the extruder screws 430 may be configured for applying compression and shear forces to the isolated cannabis trichomes 420 via a plurality of interpenetrate helicoidal surfaces present along at least a portion of the extruder screws 430.
[0117] The extruder apparatus 410 may also implement a pressure sensing element 460 at the die vicinity zone 455 which is a measure of the shear force applied on the isolated cannabis trichomes 420 packing them into a cohesive mass. The pressure may be at a value of about 1 bar or more. For example, a pressure of from about 1 bar to about 70 bar, including any ranges therein or any value therein. For example, a pressure of from about 1 bar to about 65 bar, from about 3 bar to about 60 bar, from about 4 bar to about 55 bar, from about 6 bar to about 50 bar, from about 8 bar to about 45 bar, from about 10 bar to about 40 bar, from about 12 bar to about 35 bar, from about 12 bar to about 32 bar, from about 14 bar to about 30 bar, from about 16 bar to about 28 bar, from about 18 bar to about 26 bar, or from about 20 bar to about 24 bar including any ranges therein or any value therein. For example, a pressure of about 1 bar, about 3 bar, about 4 bar, about 5 bar, about 8 bar, about 10 bar, about 12 bar, about 14 bar, about 16 bar, about 18 bar, about 22 bar, about 22 bar, about 24 bar, about 26 bar, about 28 bar, about 30 bar, about 32 bar, about 35 bar, about 40 bar, about 45 bar, about 50 bar, about 55 bar, about 60 bar, or around 65 bar.
[0118] When desired, the system 400 may also implement heating by maintaining a set of predetermined temperature within the one or more predetermined portions or zones 450A-G of the extruder apparatus 410, or throughout the length of the extruder apparatus 410, depending on specifics applications. For example, the temperature being applied within each of the one or more predetermined portions or zones 450A-G of the extruder apparatus 410 may be at a value of about 170°C or less, the temperature in one zone being selected independently from another. For example, each of the one or more predetermined portions or zones 450A-G can independently be at a temperature selected within the range of from about 20°C to about 170°C, including any ranges therein or any value therein. For example, each of the one or more predetermined portions or zones 450A-G can independently be at a temperature of about 20°C, about 25°C, about 30°C, about 35°C, about 40°C, about 45°C, about 50°C, about 55°C, about 60°C, about 65°C, about 70°C, about 80°C, about 90°C, about 100°C, about 110°C, about 120°C, about 130°C, about 140°C, about 150°C, about 160°C, or about 170°C. Also, depending on specific application, heating is also implemented at the extruder die by maintaining a predetermined temperature at the die zone 455. The system 400 may also implement several zones across the length of the apparatus 410 each performing a single functionality including but not limiting to conveying, mixing, compressing, and reversing the flow direction of the resinous mixture (or isolated cannabis trichomes). The operating parameters of the extruder apparatus 410, such as those discussed previously (e.g., temperature, pressure, and extruder screws rpm), can be selected to alter residence time of the resinous mixture (or isolated cannabis trichomes 420) in the extruder apparatus 410 to obtain the cohesive mass 480. Advantageously, it has been observed that operating parameters such as heat and extrusion speed change the pressure experienced at the die and may alter the characteristics of the hashish product discussed above. For example, the pressure applied by the extruder screws can be accompanied by different temperature settings within each portions or zones 450A-G of the extruder to enhance mixing of the isolated cannabis trichomes, extract the resinous content of the trichomes and obtain a heated, cohesive, continuous, resinous mixture, preferably substantially homogenous resinous mixture. For example, the heating and mixing can continue until a desired level of homogeneity is obtained.
[0119] In some embodiments, the heating may additionally advantageously assist in mixing the isolated cannabis trichomes 420 and optional additional components 440 to form the cohesive mass 480. For example, the heating can assist in at least partially melting optional additional components 440, such as cannabinoid isolate.
[0120] In some embodiments, the heat may be applied through heating elements (not shown) embedded with the extruder screws 430 extending along the one or more predetermined portions or zones 450A-G across the length of the extruder 410. To control the amount of heat input to the extruder and ensure that a predetermined temperature prevails in a certain zone 450A-G within the extruder 410, one or more temperature controlling units (not shown) can also be associated with the extruder apparatus 410 to monitor heat within the certain zone 450A-G of the extruder apparatus 410 and take any necessary action in the event of major deviations from the intended extrusion temperature.
[0121] At least a portion of the resinous mixture exits an extruder die 470 at the outlet of the extruder apparatus 410 in the form of an elongated, continuous solid or semi-solid cohesive mass 480. The die 470 may impart any pre-determined shape to the cohesive mass 480. At that point in the process, the long and continuous solid or semi-solid cohesive mass 480 can be subjected to ambient temperature and pressure.
[0122] A cutting means 485 may be placed downstream of the extruder die 470 to cut the cohesive mass 480 according to a pre-established cutting pattern. In a non-limiting example of implementation, the pre-established cutting pattern may comprise cutting the cohesive mass 480 along a transverse axis and at pre-determined time intervals to obtain hashish product units of a pre-determined length and/or weight. For example, to obtain a plurality of hashish product units with consistent dimensions and/or weight, the cutting means can act intermittently to cut the cohesive mass 480 into individual units of hashish product 510. The individual units of hashish product could be further transferred onto a flat conveyor belt or fall under gravity over an inclined conveyor belt (not shown) and sent for packaging and/or storage.
Test procedure for assessing %reflectance
[0123] FIG. 5 illustrates a non-limiting schematic of a system 500 for determining gloss and %reflectance of the hashish product 520 using a glossmeter 510.
[0124] The hashish product 510 may lie on a flat surface and the glossmeter 510 is placed on top of the hashish product. The glossmeter 510 has a built-in light emitter 530A that directs incident light 540A onto the surface of the hashish product with an incidence angle Y. The incidence angle Y may vary depending on the level of gloss (GU) as well as the particular industry wherein these measurements are done. As described previously, typical values for Y are 20°, 60° or 80° wherein typically, Y=20° is used for a high gloss surface (>70 GU), Y=60° is used for a semi-gloss surface (10-70 GU) and Y=85° is used for a low gloss/matt surface (<10 GU). Reflected light 540B is the light reflected from the surface of the hashish product at the same angle as the incident angle Y and is sensed by a built-in photodetector 530B. Diffuse reflected lights 550 are lights reflected in all directions with angles ¹Y. The glossmeter upon incidence of light on the surface of the hashish product 510 with the angle Y, determines the fraction of light reflected from the surface at the same angle as incident light angle (Y for 540A) to calculate gloss unit (GU) and further the %reflectance as discussed previously.
EXAMPLES
[0125] The following examples are for illustrative purposes only and are not meant to limit the scope of the compositions and methods described herein.
Comparative Example 1
[0126] In this Example, multiple batches of isolated cannabis trichomes (BBI-038, NLxBB strain) were separately loaded into the feed hopper of an ETPI Lab extruder (The Bonnot Company, USA) having a single extrusion screw. Water in different amounts was added during extrusion of each batch of isolated cannabis trichomes. The resulting hashish product from each batch was monitored for mold growth over time. The results are set forth in Table CX-1.
Table CX-1
Figure imgf000034_0001
[0127] It was observed that hashish products having a moisture content above 8 wt.% relative to total weight of the hashish product increased the likelihood of mold formation within 1-2 weeks.
[0128] Examples of hashish products made according to principles described herein are discussed below. In these examples, for each hashish product, a sample of the hashish product was prepared and tested to measure various characteristics of the hashish product, such as %reflectance, etc. The sample was prepared by flattening a portion of the hashish product for 30 seconds at a pressure of 9000 psi on a 3 in. x 5 in. area die. The %reflectance of the hashish product was determined by measuring gloss units (GU) using a LANDTEK GM-268 glossmeter set up with an 85° angle of incidence.
Example 1
[0129] In this example, a batch of isolated cannabis trichomes was processed in a twin-screw extruder to obtain a hashish product.
[0130] A batch of isolated cannabis trichomes (Meridian strain) was loaded into the feed hopper (zone 1) of a Pharma 11 twin-screw extruder (ThermoFisher Scientific™, USA) with parallel 11mm diameter twin screws and length-to-diameter ratio (L/D) of 40:1 segmented into 7 processing zones (zone 2 to zone 8). A chiller circulating water at 10°C was used to implement temperature control within the processing zones as well as the die. The initial extruder setup (I) featured two mixing zones (“MIX”) within the middle part of the extruder (i.e. , zones 4 and 6) and a compression zone (“COMP”) at the end of the screw (zone 8), as set forth in Table EX-1-1 :
Table EX-1-1
Figure imgf000035_0001
[0131] The isolated cannabis trichomes were fed in the twin-screw extruder with a feed rate of 1.7 g/min. The twin-screw extruder having a torque of 5-8%, an rpm of 300 and a 7mm die (pressure of 0-1 bar, temperature 70°C or 90°C). The temperature profile across the extruder length was according to Table EX- 1-2:
Table EX- 1-2
Figure imgf000035_0002
[0132] The resulting hashish product (see FIG. 6A) made from isolated cannabis trichomes at a die temperature of 70°C had a shredded (non-cohesive) appearance whereas increasing the die temperature to 90°C resulted in a hashish product with smooth and malleable texture that was brown in color. Without being bound by any theory, it seemed that the larger the temperature difference between the die temperature and resinous mixture temperature, the hashish product output from the die would be susceptible to more deformation. Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish product had a reflectance of 6.4 GU, corresponding to a %reflectance of 4%85.
Example 2
[0133] In this example, extruder setup (I) from Example 1 was maintained while a die with smaller diameter (4.5 mm) was employed resulting in an increase in cohesiveness and darker color of the extruded hashish product.
[0134] Isolated cannabis trichomes (Meridian strain) with a feed rate of 2.5 g/min were fed to the twin-screw extruder at an rpm of 300. The temperature profile across the extruder length was according to Table EX-2-1 :
Table EX-2-1
Figure imgf000036_0001
[0135] It was observed that decreasing the die diameter resulted in gradual clogging and pressure build up at the die, which halted the extrusion operation upon steady state. This was attributed to separation of resins from the isolated cannabis trichomes at the die (due to high temperature at the die) which resulted in the passage of resin material through the die leaving the non-viscous plant material behind the die which in turn led to clogging. Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish product had a reflectance of 7.2 GU, corresponding to a %reflectance of 4.5%85. Example 3
[0136] In this example, extruder setup (I) from Example 1 and die diameter of Example 2 (4.5 mm) were maintained while the extruder feed was 94 wt.% isolated cannabis trichomes and 4% water to further assist flow through the extruder. Also, the temperature at the die and within the mixing zones were lowered to lessen the separation of resin from the trichomes.
[0137] Isolated cannabis trichomes (Meridian strain) with a feed rate of 2.5 g/min (94 wt% isolated cannabis trichomes and 4% water) were fed to the twin-screw extruder at an rpm of 300, a 10% torque, die temperature and pressure of 80°C and 1 bar, respectively. The temperature profile across the extruder length was according to Table EX-3-1:
Table EX-3-1
Figure imgf000037_0001
[0138] It was observed that adding water to the isolated cannabis trichomes did not have a significant impact on clog prevention (as compared to Example 2) and only delayed the clogging after reaching steady state by ~30 minutes. The combined feeding of water and isolated cannabis trichomes also resulted in a clumpy mix that further contributed to clogging. Moreover, the separation of resins from the isolated cannabis trichomes at the die (due to high temperature at the die) repeated and the resulting hashish product was less pliable (harder) as compared to the hashish product obtained in Example 2. Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish product had a reflectance of 6.5 GU, corresponding to a %reflectance of 4%85.
Example 4
[0139] In this example, identical process parameters as those of Example 3 were implemented except that water was not added in the feed stream. Also, to analyze the effects of torque, die temperature, die pressure and temperature across extruder zones on the hashish product, these conditions were also varied in this example. [0140] Isolated cannabis trichomes (Meridian strain) with a feed rate of 2.5 g/min were fed to the twin-screw extruder at a reduced rpm of 100 and under the following conditions as set forth in Tables EX-4-1 to EX-4-3:
[0141] Operating condition I)
Table EX-4-1
Figure imgf000038_0001
[0142] Operating condition II)
Table EX-4-2
Figure imgf000038_0002
[0143] Operating condition III)
Table EX-4-3
Figure imgf000038_0003
[0144] It was observed that increased temperature in mixing zones (operating condition I vs. Ill) or die (operating condition II vs. Ill) decreased the required mechanical work (as evidenced by torque and die pressure) to extrude the isolated cannabis trichomes and output the hashish product. Meanwhile, the colors of the obtained hashish products across operating conditions I) to III) varied from beige/brown to dark brown albeit, all products lacked the desirable shininess. Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish products corresponding to EX-4-1 to EX-4-3 had reflectance values of 7.7 GU, 6.9 GU and 6.8 GU, respectively, corresponding to %reflectance values of 4.8%85, 4.3%85 and 4.2%85, respectively.
[0145]
Example 5
[0146] In this example, extruder setup (I) from Example 1 was maintained. However, in order to achieve a shiny hashish product, it was postulated to increase the mechanical work by decreasing the die diameter to 2 mm thus generating more pressure. Also, to analyze the effects of extruder rpm and zone temperatures on the hashish product, these conditions were varied in this example.
[0147] Isolated cannabis trichomes (Meridian strain) with a feed rate of 2.5 g/min were fed to the twin-screw extruder under the following conditions as set forth in Tables EX- 5-1 to EX- 5-3 (variable zone temperatures in bold):
[0148] Operating condition I)
Table EX-5-1
Figure imgf000039_0001
[0149] Operating condition II)
Table EX-5-2
Figure imgf000039_0002
[0150] Operating condition III) Table EX-5-3
Figure imgf000040_0001
[0151] It was observed from operating condition I) that feeding the isolated cannabis trichomes to the extruder at 50 rpm resulted in low product clearance from the screws and therefore, hashish product output was inconsistent (undesirable). While increased rpms resulted in more steady output of hashish product, all products lacked the desirable shine. It was concluded that the rpm must be adjusted to the feed rate to allow sufficient clearance of the material in order to avoid problems in feeding (such as bridging). It was postulated that an increase in retention time of isolated cannabis trichomes in the mixing zone (more mechanical and thermal energy transfer) would contribute to more desirable hashish product. Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish products corresponding to EX- 5-1 to EX-5-3 had reflectance values of 6.8 GU, 6.9 GU and 7.3 GU, respectively, corresponding to %reflectance values of 4.2%85, 4.3%85 and 4.6%85, respectively.
Example 6
[0152] In this example, an additional extruder setup (II) was tested. Extruder setup (II) distinguishes from extruder setup (I) in the presence of a reverse flow segment (“REV”) after the first mixing zone with the aim of increasing retention time of isolated cannabis trichomes in the mixing zone (more mechanical and thermal energy transfer). The overall breakdown for the extruder setup (II) is set forth in Table EX-6-1 :
Table EX-6-1
Figure imgf000040_0002
[0153] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2.5 g/min were fed to the twin-screw extruder and under the following conditions as set forth in Tables EX-6-2 to EX-6-5 to assess the impact of change in screw step and temperature variation at the die and within different zones:
[0154] Operating condition I)
Table EX-6-2
Figure imgf000041_0001
[0155] Operating condition II)
Table EX-6-3
Figure imgf000041_0002
[0156] Operating condition III)
Table EX-6-4
Figure imgf000041_0003
[0157] Operating condition IV)
Table EX-6-5
Figure imgf000041_0004
[0158] It was observed from operating conditions I) to IV) that the obtained hashish products were darker in color and more malleable compared to those obtained in Examples 1 to 5 that employed the initial screw setup (I) without a reverse flow element. Further, comparing the hashish products obtained across operating conditions I) to IV) of this Example, the surface of the hashish product from operating condition IV) was less smooth and less shiny compared to that of operating condition III). Hashish product obtained from operating condition III) was the only one exhibiting shiny characteristic. The overall improvement in product characteristics in this Example compared to previous Examples was attributed to increased residence time (due to addition of reverse flow element). Also, the observed increase in compaction within the mixing zones seemed to be due to an increase in heat and mechanical energy transfer to the isolated cannabis trichomes with the extruder setup (II). Further, increase of temperature in variable zones (from 80°C to 140°C) showed to have a positive impact on hashish product quality (in terms of appearance) up to a certain point beyond which a degradation was observed. For example, under the conditions assessed here, this point was about 120°C.
[0159] Overall, it was concluded that extending the duration through which the isolated cannabis trichomes are subjected to compression and shear forces within the screw path would lead to hashish products with higher quality (specifically in terms of appearance). The appearance characteristics are shown in FIG. 6B (corresponding to operating conditions III) and IV)). Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish products corresponding to EX-6-3 to EX-6-5 had reflectance values of 6.5 GU, 7.1 GU and 7.2 GU, respectively, corresponding to %reflectance values of 4%85, 4.4%85 and 4.5%85, respectively).
Example 7
[0160] In this example, an additional extruder setup (III) was tested. Extruder setup (III) distinguishes from extruder setup (II) in the presence of a second compression element after the lead element while the two mixing sections were combined upstream of the reverse flow element. The mixing section was placed near the compression elements, spanning the last two heated zones as set forth in Table EX-7-1 : Table EX-7-1
Figure imgf000043_0001
[0161] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min were fed to the twin-screw extruder and under the following conditions as set forth in Tables EX-7-2 to EX-7-5 to assess the impact of change in screw step and temperature variation at the die and within variable zones:
[0162] Operating condition I)
Table EX-7-2
Figure imgf000043_0002
[0163] Operating condition II)
Table EX-7-3
Figure imgf000043_0003
[0164] Operating condition III)
Table EX-7-4
Figure imgf000043_0004
[0165] Operating condition IV)
Table EX-7-5
Figure imgf000044_0001
[0166] It was observed from operating conditions I) to IV) that the obtained hashish product from operating condition IV) was less shiny and less smooth (i.e., deformation on the surface of the product) compared to that obtained from operating condition III) which was in turn found to be less shiny and less smooth compared to that obtained from operating condition II). Moreover, the hashish product from operating condition IV) was pushed out of the die in an inconsistent manner with black resin dripping from the die (characteristic of a pre-clog event). Overall, it was concluded that by using appropriate temperature within zones that have increased product compaction and shear, it would be possible to obtain a hashish product with desired characteristics (color and malleability). For example, under the conditions assessed here, the preferred temperature range was from about 100°C to about 120°C. It is hypothesized that the product could be made further soft and malleable by increasing the shear forces experienced by the product via the elongation of compression and mixing segments or via an increase in retention time within the mixing segments. Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish products corresponding to EX-7-2 to EX-7-5 had reflectance values of 6.9 GU, 7.1 GU, 7.3 GU and 7.1 GU, respectively, corresponding to %reflectance values of 4.3%85, 4.4%85, 4.5%85 and 4.4%85, respectively.
Example 8: Extruded Hash Infused with CBD Distillate
[0167] In this Example, hashish product infused with CBD was manufactured using the extruder set up (II) as set forth in Table EX-8-1. Table EX-8-1
Figure imgf000045_0001
[0168] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min were fed to the twin-screw extruder. CBD distillate was introduced via a liquid feeding port in zone 3 through use of a syringe that dispensed the molten product at 60°C at a programmed feed rate. The extruder was operated with the following operating conditions as set forth in Tables EX-8-2, EX-8-4 and EX-8-6:
[0169] Operating condition I): control with no CBD distillate infusion
Table EX-8-2
Figure imgf000045_0002
[0170] Analytical results of input isolated cannabis trichomes and output hash corresponding to operating condition I) are shown in Table EX-8-3 (n=15 samples of isolated cannabis trichomes and hashish products). CBD and THC levels were measured with high performance liquid chromatography (HPLC) while moisture content was determined via Thermogravimetric Moisture Balance-type Analyzer.
Table EX-8-3
Figure imgf000046_0001
s = Standard Deviation, CV= Coefficient of Variation [0171] Operating condition II) - CBD distillate infusion
Table EX-8-4
Figure imgf000046_0002
[0172] Analytical results of input isolated cannabis trichomes and output hash corresponding to operating condition II) are shown in Table EX-8-5 (n=15 samples of isolated cannabis trichomes and hashish products). CBD and THC levels were measured with high performance liquid chromatography (HPLC) while moisture content was determined via Thermogravimetric Moisture Balance-type Analyzer:
Table EX-8-5
Figure imgf000046_0003
[0173] Operating condition III) - CBD distillate infusion
Table EX-8-6
Figure imgf000047_0001
It was visually observed that the addition of molten distillate resulted in a homogenous and shiny hashish product while causing a reduction in torque and die pressure (operating condition I vs II) due to the lubricating effect during extrusion. Moreover, the moisture content of the hashish product under operating condition II) that entailed distillate addition was lower than that of operating condition I) wherein only isolated cannabis trichomes were fed to the extruder. In conclusion, CBD infusion during extrusion could be done in a homogenous manner and resulted in a shinier and more malleable hashish product. Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish products corresponding to EX-8-2 and EX-8-4 had reflectance values of 7.5 GU and 7.7 GU, respectively, corresponding to %reflectance values of 4.6%85 and 4.8%85, respectively.
Example 9: Extruded Hash Infused with CBD Isolate
[0174] In this example, hashish product infused with CBD isolate was manufactured in order to compare the resulting hashish product characteristics with that of Example 8. Same extruder setup (II) as that one of Example 8 was used.
[0175] Isolated cannabis trichomes (NLxBB strain) and CBD isolate were mixed using a commercially available KitchenAid™ mixer and the mixture was fed to the twin-screw extruder at a rate of 2 g/min and under the following operating conditions as set forth in Tables EX- 9-1 to EX- 9-2: [0176] Operating condition I): control with no CBD isolate infusion
Table EX-9-1
Figure imgf000048_0001
[0177] Operating condition II) - CBD isolate infusion
Table EX-9-2
Figure imgf000048_0002
[0178] Analytical results of input isolated cannabis trichomes and output hash corresponding to operating condition II) are shown in Table EX- 9-3 (n=15 samples of isolated cannabis trichomes and hashish products). CBD and THC levels were measured with high performance liquid chromatography (HPLC) while moisture content was determined via Thermogravimetric Moisture Balance-type Analyzer:
Table EX-9-3
Figure imgf000048_0003
[0179] It was visually observed that the addition of CBD isolate to isolated cannabis trichomes and feeding them as a mixture to the twin-screw extruder resulted in a lower torque and die pressure as the CBD isolate melted during extrusion and seemingly provided lubrication to the extruding material. Like Example 8, the resulting hashish product upon addition of CBD isolate was a shinier, softer and more malleable hashish product compared to the control hashish product obtained from operating condition I). Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish products corresponding to EX-9-1 and EX-9-2 had reflectance values of 7.4 GU and 7.9 GU, respectively, corresponding to %reflectance values of 4.6%85 and 4.9%85, respectively.
Example 10: Extruded Hash Infused with CBD Distillate
[0180] In this Example, hashish product infused with CBD was manufactured using Extruder setup (III) from Example 7.
[0181] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min were fed to the twin-screw extruder. CBD distillate was introduced via a liquid feeding port in zone 3 through use of a syringe that dispensed the molten product at 60°C at a programmed feed rate. The extruder was operated with the following operating conditions as set forth in Tables EX-10-1, EX-10-3, EX- 10-5 and EX- 10-6:
[0182] Operating condition I): control with no CBD distillate infusion
Table EX- 10-1
Figure imgf000049_0001
[0183] Analytical results of THCA to THC conversion for input isolated cannabis trichomes and output hash corresponding to operating condition I) are shown in Table EX-10-2 (n=15 samples of isolated cannabis trichomes and hashish products). THCA and THC levels were measured with high performance liquid chromatography (HPLC): Table EX- 10-2
Figure imgf000050_0001
s = Standard Deviation, CV= Coefficient of Variation [0184] Operating condition II) - CBD distillate infusion
Table EX- 10-3
Figure imgf000050_0002
[0185] Analytical results of THCA to THC conversion for input isolated cannabis trichomes and output hash corresponding to operating condition II) are shown in Table EX-10-4 (n=15 samples of isolated cannabis trichomes and hashish products). THCA and THC levels were measured with high performance liquid chromatography (HPLC):
Table EX- 10-4
Figure imgf000050_0003
o = Standard Deviation, CV= Coefficient of Variation [0186] Operating condition III) - CBD distillate infusion Table EX- 10-5
Figure imgf000051_0001
[0187] Operating condition IV) - CBD distillate infusion
Table EX- 10-6
Figure imgf000051_0002
[0188] It was visually observed that the control samples (without addition of distillate) were tougher (yet malleable) compared to those sample obtained with added distillate. Increasing the amount of added distillate resulted in softer and shinier hashish product. As for the extruder, it was observed that the addition of distillate beyond 0.5 g/min had no significant effect on die pressure. Moreover, the extrudate hashish products obtained under operating conditions III) and IV) were less smooth compared to those obtained under operating conditions I) and II) which had no or less distillate added. Finally, the conversion of THCA to THC during extrusion was observed to be less significant when infusing the product with distillate. The appearance characteristics are shown in FIG. 6D. Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish products corresponding to EX-10-1, EX-10-3, EX-10-5 and EX-10-6 had reflectance values of 7.4 GU, 7.9 GU, 8.8 GU and 8.9 GU, respectively, corresponding to %reflectance values of 4.6%85, 4.9%85, 5.5%85 and 5.6%85, respectively. [0189] Also, without being bound by any theory, the present inventor believes that there is a change in product flow through the die upon increase in distillate feeding as the product softens and that the hashish product needs to exit the die at a cooler temperature in order to remain smooth
Example 11: Extruded Hash Infused with CBD Distillate
[0190] In this Example, the screw setup (III) from Example 10 was maintained and the die diameter was changed from 2mm to 4.5mm.
[0191] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min were fed to the twin-screw extruder. CBD distillate was introduced via a liquid feeding port in zone 3 through use of a syringe that dispensed the molten product at 60°C at a programmed feed rate. The extruder was operated with the following operating conditions as set forth in Tables EX-11-1 to EX-11-3:
[0192] Operating condition I): control with no CBD distillate infusion
Table EX-11-1
Figure imgf000052_0001
Figure imgf000052_0006
Figure imgf000052_0007
[0193] Operating condition II) - CBD distillate infusion
Table EX- 11-2
Figure imgf000052_0002
Figure imgf000052_0003
Figure imgf000052_0004
Figure imgf000052_0005
[0194] Operating condition III) - CBD distillate infusion Table EX- 11-3
Figure imgf000053_0001
Figure imgf000053_0002
Figure imgf000053_0003
[0195] It was visually observed that the control hashish products (operating condition I)) were malleable and had a shiny black and smooth appearance. However, they were tougher compared to the hashish product from operating condition II) which were in turn tougher than those obtained from operating condition III). In fact, hashish products obtained under operating condition III) was less smooth as it was becoming increasingly soft due to increase in distillate feed rate. The appearance characteristics are shown in FIG. 6E (corresponding to operating conditions I) to III)). Interestingly, no mold has formed on the hashish products made in this example over a period of at least 2 weeks. The hashish products were kept in sealed Ziploc™ bags, placed in a plastic container, at room temperature with exposure to daylight. The hashish products corresponding to EX-11-1 , EX-11-2 and EX-11-3 had reflectance values of 7.3 GU, 8.7 GU and 8.7 GU, respectively, corresponding to %reflectance values of 4.5%85, 5.4%85 and 5.4%85, respectively.
[0196]
Example 12
[0197] In this Example, hashish products are manufactured using a kief batch from Meridian strain by three distinct methods of extrusion with a twin-screw extruder (Pharma 11 twin-screw extruder (ThermoFisher Scientific™, USA), extrusion with single-screw extruder (ETPI Lab extruder - Bonnot Company, USA as described for example in PCT/CA2021/050673) and pressing with an industrial press (for example as described in PCT/CA2020/051733). The following operating conditions were used in each case, as set forth in Table EX-12-1. Table EX- 12-1
Figure imgf000054_0001
Figure imgf000054_0002
Figure imgf000054_0003
[0198] The resulting products in terms of appearance are shown in FIG. 7. It was visually observed that the pressed hashish product (operating condition III) had a light color with darker patches scattered over the surface (i.e., heterogeneous appearance likely due to heterogeneous distribution of cannabis plant matter). Although the hashish product obtained from the single screw extruder (operating condition II) had a relatively more consistent and brown color, it lacked shininess. In contrast, the hashish product obtained from the twin-screw extruder (operating condition I) had both a consistent black color and a shiny surface.
[0199] High potency kief can make shiny hash more easily than low potency hash as it is easier bring out the resin to the surface. Hash that has been post-processed to impart better surface uniformity, such as when rolling into a ball, will also make any hash shinier. When enough resin coats the surface of the kief-turned-hash and the hash also meets the criteria of a smooth surface, it will have gloss. Higher potency can be obtained when making hash from trichomes isolated with water and ice methods (i.e., “bubble hash”), which have less impurities and higher potency. Dry sift kief, in contrast, necessitates a lot of mechanical and/or thermal energy to get that shine / gloss. The present inventors have demonstrated that with the process described herein, which preferably uses a twin-screw extruder, there is sufficient energy input when mixing any type of kief, such as low potency, dry sift kief, etc., to facilitate resin oozing out from the trichomes and imparting better characteristics to the hashish product.
[0200] Other examples of implementations will become apparent to the reader in view of the teachings of the present description and as such, will not be further described here.
[0201] Note that titles or subtitles may be used throughout the present disclosure for convenience of a reader, but in no way, these should limit the scope of the invention. Moreover, certain theories may be proposed and disclosed herein; however, in no way they, whether they are right or wrong, should limit the scope of the invention so long as the invention is practiced according to the present disclosure without regard for any particular theory or scheme of action.
[0202] All references cited throughout the specification are hereby incorporated by reference in their entirety for all purposes.
[0203] Reference throughout the specification to “some embodiments”, and so forth, means that a particular element (e.g., feature, structure, and/or characteristic) described in connection with the invention is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the described inventive features may be combined in any suitable manner in the various embodiments.
[0204] It will be understood by those of skill in the art that throughout the present specification, the term “a” used before a term encompasses embodiments containing one or more to what the term refers. It will also be understood by those of skill in the art that throughout the present specification, the term “comprising”, which is synonymous with “including,” “containing,” or “characterized by,” is inclusive or open-ended and does not exclude additional, un-recited elements or method steps.
[0205] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. In the case of conflict, the present document, including definitions will control.
[0206] As used in the present disclosure, the terms “around”, “about” or “approximately” shall generally mean within the error margin generally accepted in the art, such as for example +/- 20%, +/- 15%, +/- 10%, or +/- 5%. Hence, numerical quantities given herein generally include such error margin such that the terms “around”, “about” or “approximately” can be inferred if not expressly stated.
[0207] As used throughout the present disclosure, the terms "concentration" and "content" are used interchangeably and refer to the weight or mass fraction of a constituent, i.e., the weight or mass of a constituent divided by the total mass of all constituents, and is expressed in wt.%, unless stated otherwise.
[0208] Although various embodiments of the disclosure have been described and illustrated, it will be apparent to those skilled in the art considering the present description that numerous modifications and variations can be made. The scope of the invention is defined more particularly in the appended claims.

Claims

1. A process of making a hashish product, comprising a) providing isolated cannabis trichomes; b) mixing the isolated cannabis trichomes while adding mechanical or thermal energy under conditions sufficient to obtain a resinous mixture; and c) retrieving at least a portion of the resinous mixture through an extrusion die to obtain the hashish product, wherein the hashish product is a substantially homogeneous cohesive mass of the isolated trichomes having a % reflectance of at least 4%85.
2. The process according to claim 1, wherein the hashish product has a lightness value L* £ 50 on CIELAB scale, preferably from 0 to about 40, or of from about 10 to about 30, or of from about 15 to about 25.
3. The process according to claim 1 or 2, wherein the hashish product has a % reflectance of at least 4.5%85, at least 5%85, or at least 5.5%85.
4. The process according to any one of claims 1 to 3, wherein the mixing includes applying compression and shear forces to the isolated trichomes via a plurality of interpenetrate helicoidal surfaces within an elongated enclosure.
5. The process according to claim 4, wherein the interpenetrate helicoidal surfaces are on at least two screws extending along at least a portion of a longitudinal axis of the elongated enclosure.
6. The process according to claim 5, the process further comprising adjusting a rotational speed of the at least two screws to obtain the resinous mixture.
7. The process according to claim 6, wherein the rotational speed of the at least two screws is between about 10 rpm and about 1000 rpm, preferably between 100 rpm and 200 rpm.
8. The process according to any one of claims 5 to 7, wherein said elongated enclosure comprises a plurality of sections corresponding to longitudinal segments of the at least two screws.
9. The process according to claim 8, the process further comprising controlling a temperature in at least one section of the plurality of sections.
10. The process according to claim 9, wherein the temperature in each section of the plurality of sections is independently selected in the range of from about 20°C to about 170°C.
11. The process according to any one of claims 8 to 10, wherein the plurality of sections includes at least one mixing section and at least one conveying section.
12. The process according to claim 11, wherein the at least one mixing section is maintained at a first temperature and the least one conveying section is maintained at a second temperature, the first and second temperatures being different.
13. The process according to any one of claims 8 to 12, wherein the plurality of sections includes at least one reverse flow section.
14. The process according to any one of claims 8 to 13, wherein at least a first section of the plurality of sections comprises a first inlet for providing the isolated trichomes.
15. The process according to claim 14, wherein at least a second section of the plurality of sections comprises a second inlet for providing one or more additional component(s).
16. The process according to claim 15, wherein the one or more additional component(s) include one or more cannabinoid, one or more terpene, one or more flavonoid, one or more flavoring agent, water, one or more non-toxic coloring agent, or a mixture thereof.
17. The process according to claim 16, wherein the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
18. The process according to claim 16 or 17, wherein the one or more cannabinoid(s) includes a plurality of cannabinoids.
19. The process according to any one of claims 16 to 18, wherein the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
20. The process according to any one of claims 1 to 19, further comprising cutting the hashish product according to a pre-established cutting operational parameter.
21. The process according to claim 20, wherein the cutting pattern includes cutting the hashish product along a transverse axis to obtain pieces thereof of identical length and/or weight.
22. The process according to any one of claims 1 to 21 , wherein the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%.
23. The process according to any one of claims 1 to 22, wherein the isolated cannabis trichomes are from a single cannabis strain.
24. The process according to any one of claims 1 to 22, wherein the isolated cannabis trichomes are from a plurality of cannabis strains.
25. The process according to any one of claims 1 to 24, wherein the hashish product comprises a moisture content of no more than about 8 wt.%, such as from about 2 wt.% to about 8 wt.%, preferably from about 2 to about 5 wt.%, determined via Thermogravimetric Moisture Balance-type Analyzer.
26. The process according to any one of claims 1 to 25, wherein the isolated trichomes are dry- sift kief.
27. A hashish product comprising a substantially homogeneous cohesive mass of isolated cannabis trichomes made by the process according to any one of claims 1 to 25.
28. A hashish product comprising a substantially homogeneous cohesive mass of isolated cannabis trichomes having a % reflectance of at least 4%85.
29. The hashish product according to claim 28, wherein the hashish product has a lightness value L* £ 50 on CIELAB scale, or a lightness value L* from 0 to about 40, of from about 10 to about 30, of from about 15 to about 25.
30. The hashish product according to claim 28 or 29, wherein the hashish product has a % reflectance of at least 4.5%85, at least 5%85, or at least 5.5%85.
31. The hashish product according to any one of claims 28 to 30, comprising one or more additional component(s) selected from one or more cannabinoid, one or more terpene, one or more flavonoid, one or more flavoring agent, one or more non-toxic coloring agent, and any mixtures thereof.
32. The hashish product according to claim 31, wherein the one or more cannabinoid(s) is in the form of a crude cannabis extract, a cannabis isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter, or any combination thereof.
33. The hashish product according to claim 31 or 32, wherein the one or more cannabinoid(s) includes a plurality of cannabinoids.
34. The hashish product according to any one of claims 31 to 33, wherein the one or more cannabinoid(s) includes tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), or any combinations thereof.
35. The hashish product according to any one of claims 28 to 34, wherein the hashish product comprises a cannabinoid content of from about 5 wt.% to about 90 wt.%.
36. The hashish product according to any one of claims 28 to 35, wherein the isolated cannabis trichomes are from a single cannabis strain.
37. The hashish product according to any one of claims 28 to 35, wherein the isolated cannabis trichomes are from a plurality of cannabis strains.
38. The hashish product according to any one of claims 28 to 37, wherein the hashish product comprises a moisture content of no more than about 8 wt.%, such as from about 2 wt.% to about 8 wt.%, preferably of from about 2 wt.% to about 5 wt.%, determined via Thermogravimetric Moisture Balance-type Analyzer.
39. The hashish product according to any one of claims 28 to 38, wherein the isolated trichomes are dry-sift kief.
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